CN111036182A - Preparation of uranium adsorption gel balls based on aluminum sludge and method for treating uranium-containing wastewater - Google Patents
Preparation of uranium adsorption gel balls based on aluminum sludge and method for treating uranium-containing wastewater Download PDFInfo
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- CN111036182A CN111036182A CN202010016216.2A CN202010016216A CN111036182A CN 111036182 A CN111036182 A CN 111036182A CN 202010016216 A CN202010016216 A CN 202010016216A CN 111036182 A CN111036182 A CN 111036182A
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- 229910052770 Uranium Inorganic materials 0.000 title claims abstract description 211
- JFALSRSLKYAFGM-UHFFFAOYSA-N uranium(0) Chemical compound [U] JFALSRSLKYAFGM-UHFFFAOYSA-N 0.000 title claims abstract description 211
- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 125
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 125
- 239000010802 sludge Substances 0.000 title claims abstract description 115
- 238000001179 sorption measurement Methods 0.000 title claims abstract description 103
- 239000002351 wastewater Substances 0.000 title claims abstract description 71
- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title claims abstract description 20
- 239000000203 mixture Substances 0.000 claims abstract description 41
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000000843 powder Substances 0.000 claims abstract description 32
- 230000010355 oscillation Effects 0.000 claims abstract description 21
- 239000004372 Polyvinyl alcohol Substances 0.000 claims abstract description 20
- 229920002451 polyvinyl alcohol Polymers 0.000 claims abstract description 20
- IXPNQXFRVYWDDI-UHFFFAOYSA-N 1-methyl-2,4-dioxo-1,3-diazinane-5-carboximidamide Chemical compound CN1CC(C(N)=N)C(=O)NC1=O IXPNQXFRVYWDDI-UHFFFAOYSA-N 0.000 claims abstract description 16
- 235000010413 sodium alginate Nutrition 0.000 claims abstract description 16
- 239000000661 sodium alginate Substances 0.000 claims abstract description 16
- 229940005550 sodium alginate Drugs 0.000 claims abstract description 16
- 238000001035 drying Methods 0.000 claims abstract description 13
- 238000003756 stirring Methods 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 12
- 238000001816 cooling Methods 0.000 claims abstract description 6
- 239000012153 distilled water Substances 0.000 claims abstract description 6
- 238000000227 grinding Methods 0.000 claims abstract description 6
- 238000010438 heat treatment Methods 0.000 claims abstract description 6
- 239000008367 deionised water Substances 0.000 claims description 10
- 229910021641 deionized water Inorganic materials 0.000 claims description 10
- 239000012535 impurity Substances 0.000 claims description 6
- 230000007935 neutral effect Effects 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 239000001110 calcium chloride Substances 0.000 claims description 5
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 5
- 238000000746 purification Methods 0.000 claims description 5
- 238000007789 sealing Methods 0.000 claims description 5
- 238000007873 sieving Methods 0.000 claims description 5
- 238000007605 air drying Methods 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 abstract description 10
- 239000003463 adsorbent Substances 0.000 abstract description 8
- 238000010923 batch production Methods 0.000 abstract description 2
- 238000003760 magnetic stirring Methods 0.000 abstract 1
- 238000009777 vacuum freeze-drying Methods 0.000 abstract 1
- 150000002500 ions Chemical class 0.000 description 8
- 239000004411 aluminium Substances 0.000 description 7
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 5
- 238000004064 recycling Methods 0.000 description 5
- BHPQYMZQTOCNFJ-UHFFFAOYSA-N Calcium cation Chemical compound [Ca+2] BHPQYMZQTOCNFJ-UHFFFAOYSA-N 0.000 description 4
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910001424 calcium ion Inorganic materials 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 238000001514 detection method Methods 0.000 description 4
- 239000008394 flocculating agent Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 229910052742 iron Inorganic materials 0.000 description 3
- NMCUIPGRVMDVDB-UHFFFAOYSA-L iron dichloride Chemical compound Cl[Fe]Cl NMCUIPGRVMDVDB-UHFFFAOYSA-L 0.000 description 3
- 239000002699 waste material Substances 0.000 description 3
- 238000004065 wastewater treatment Methods 0.000 description 3
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 2
- 150000001224 Uranium Chemical class 0.000 description 2
- 239000010949 copper Substances 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 2
- 230000002452 interceptive effect Effects 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 229910017604 nitric acid Inorganic materials 0.000 description 2
- 230000000630 rising effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- -1 uranyl ions Chemical class 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 1
- 241000199919 Phaeophyceae Species 0.000 description 1
- JAQXDZTWVWLKGC-UHFFFAOYSA-N [O-2].[Al+3].[Fe+2] Chemical compound [O-2].[Al+3].[Fe+2] JAQXDZTWVWLKGC-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 150000007513 acids Chemical class 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 150000001450 anions Chemical class 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 description 1
- 150000001768 cations Chemical class 0.000 description 1
- 238000009388 chemical precipitation Methods 0.000 description 1
- 239000004927 clay Substances 0.000 description 1
- 230000001112 coagulating effect Effects 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000003795 desorption Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 150000004676 glycans Chemical class 0.000 description 1
- 239000003673 groundwater Substances 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 238000012690 ionic polymerization Methods 0.000 description 1
- 238000005272 metallurgy Methods 0.000 description 1
- 238000005065 mining Methods 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000010979 pH adjustment Methods 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 230000001699 photocatalysis Effects 0.000 description 1
- 238000007747 plating Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001282 polysaccharide Polymers 0.000 description 1
- 239000005017 polysaccharide Substances 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000002285 radioactive effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 229920006395 saturated elastomer Polymers 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000002689 soil Substances 0.000 description 1
- 238000002798 spectrophotometry method Methods 0.000 description 1
- 239000002352 surface water Substances 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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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- 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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/24—Naturally occurring macromolecular compounds, e.g. humic acids or their derivatives
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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
- B01J20/22—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising organic material
- B01J20/26—Synthetic macromolecular compounds
- B01J20/261—Synthetic macromolecular compounds obtained by reactions only involving carbon to carbon unsaturated bonds
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- 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
- B01J20/28016—Particle form
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/28047—Gels
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- G21F9/00—Treating radioactively contaminated material; Decontamination arrangements therefor
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- B01J2220/00—Aspects relating to sorbent materials
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Abstract
The preparation method of uranium adsorption gel balls based on aluminum sludge and the method for treating uranium-containing wastewater comprise the following steps of firstly washing, drying, grinding and crushing the aluminum sludge; secondly, dissolving polyvinyl alcohol in distilled water, heating, magnetically stirring and cooling, adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring; then adding CaCl with the mass fraction of 3 percent when the mixture after magnetic stirring is in a sticky state2The solution is solidified into a gel ball shape; finally, the mixture in the shape of the gel ball is washed to remove CaCl on the surface2And carrying out vacuum freeze drying to obtain the uranium adsorption gel ball. When in use, the pH value of the uranium-bearing wastewater to be treated is adjusted to 4-6 according toAnd adding uranium adsorption gel balls according to the proportion of 0.4-0.8 g/L, setting the reaction time to be 0.5-6 h, the temperature to be 15-35 ℃, and the shaking table oscillation frequency to be 160 r/min. The uranium adsorption gel ball of the aluminum sludge has the advantages of simple preparation process, low cost, good adsorbent, easy realization of batch production and larger market application prospect.
Description
Technical Field
The invention relates to the technical field of uranium mining and metallurgy, in particular to a method for preparing uranium adsorption gel balls based on aluminum sludge and treating uranium-containing wastewater.
Background
With the advent of the industrial age, the ecological environment in which humans live is also destroyed, and environmental governance is an urgent problem to be solved. The exploitation of uranium ores and the development of nuclear weapons cause severe nuclear pollution. Uranium-bearing wastewater has affected the quality of surface water, ground water and organisms in its soil. Uranium, being radioactive to living organisms, enters the body through the food chain causing damage such as canceration. Therefore, the development and research of uranium-containing wastewater treatment technology are also of great importance. The uranium-bearing waste water treatment technology comprises methods such as chemical precipitation, solution extraction, photocatalysis, ion exchange and adsorption, and compared with other methods, the adsorption method has the characteristics of high efficiency, simple method, low cost, cyclic utilization, no secondary pollution and the like, and is widely used. Most of the adsorbents are in a powder state, but in actual industrial application, the powder adsorbents have the defects of difficulty in solid-liquid separation, difficulty in recovery and the like, can cause the problem of loss of recycling, are not suitable for uranium-containing wastewater treatment, so a forming technology is applied to synthesis of the adsorbents, and are more beneficial to removing uranyl ions in wastewater.
The aluminum sludge is a byproduct generated when the water body is purified by utilizing the coagulating sedimentation technology, and as a flocculating agent for purifying the water body is mostly composed of aluminum salt or aluminum polymer, the aluminum sludge not only has the property of clay, but also has the characteristic of aluminum iron oxide. At present, the aluminum sludge is mainly treated by landfill, incineration and the like by wastes, which can cause environmental pollution to a certain extent.
The polyvinyl alcohol (PVA) has the advantages of a large number of hydroxyl groups attached to the surface, good biocompatibility, no toxicity, low cost, high mechanical strength and the like, and is widely applied to the preparation of forming adsorption materials. Sodium Alginate (SA) is a sodium salt formed by ionic polymerization of polysaccharides extracted from brown algae, and is considered as a natural adsorbent due to having carboxyl (-COOH) and hydroxyl (-OH) groups. At present, gel balls formed by sodium alginate and calcium ions are widely applied to adsorption of heavy metal ions. However, the adsorption process has the defect of easy expansion due to poor mechanical properties; especially in the case of strong acids, Ca2+And H+The replacement of (a) can disrupt the network structure of the gel spheres, leading to decomposition of the gel spheres.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for preparing uranium adsorption gel spheres and treating uranium-containing wastewater based on aluminum sludge.
The technical scheme of the invention is as follows: the preparation of the uranium adsorption gel ball based on the aluminum sludge comprises the following steps,
A. pretreatment of aluminum sludge
Taking the aluminum sludge obtained after water purification in a water plant, washing surface impurities of the aluminum sludge by using deionized water, then placing the aluminum sludge in a forced air drying oven at 100-150 ℃ for 6-8 h, grinding and crushing the dried aluminum sludge to obtain aluminum sludge powder, sieving the aluminum sludge powder by using a 100-mesh sieve, and sealing and storing the aluminum sludge powder for later use.
B. Preparation of the aqueous Sol solution
Dissolving polyvinyl alcohol in distilled water, heating and magnetically stirring until the polyvinyl alcohol is completely dissolved, cooling, sequentially adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring until the mixture is uniformly mixed; wherein, the weight ratio of polyvinyl alcohol: aluminum sludge powder: the mass fraction ratio of the sodium alginate is 1: 1.5-3: 0.5 to 1.
C. Preparation of uranium adsorption gel balls
After the mixture is magnetically stirred, the mixture is in a sticky state according to the ratio of the mixture to CaCl2The mass ratio of the solution is 1: 10-30 percent of CaCl with the mass fraction of 3 percent2Injecting and extruding the solution into the mixture, and curing for 30-45 min until the mixture is in a gel ball shape.
D. Drying of uranium adsorbed gel spheres
Washing the gel-ball mixture with deionized water and anhydrous ethanol for several times until the solution is neutral, and removing CaCl on the surface2And then placing the mixture in a vacuum freeze dryer at the temperature of 20 ℃ below zero for drying for 12 hours to prepare the uranium adsorption gel balls.
The invention provides a method for treating uranium-containing wastewater by uranium adsorption gel balls based on aluminum sludge, wherein the concentration of uranium in the uranium-containing wastewater is 2-25 mg/L, the pH value is 2-8, the method comprises the following steps,
adjusting the pH value of the uranium-containing wastewater to 4-6, then adding uranium adsorption gel balls based on aluminum sludge according to the addition amount of 0.4-0.8 g/L, wherein the adsorption adopts a constant-temperature shaking table to oscillate and react for 0.5-6 h, the constant-temperature adsorption temperature is 15-35 ℃, and the oscillation frequency of the constant-temperature shaking table is 160 r/min. .
Compared with the prior art, the invention has the following characteristics:
1. the method utilizes the characteristics of three materials, namely the aluminum sludge, the polyvinyl alcohol and the sodium alginate to prepare the spherical uranium adsorbent with three-dimensional structure, can treat the uranium-containing wastewater with low concentration, utilizes the main material, namely the aluminum sludge, as an environment-friendly measure for treating wastes with processes of wastes against one another, has the characteristics of readily available raw materials, low cost and simple preparation of the adsorbent, and is easy to realize batch production.
2. After the uranium-bearing wastewater with low concentration is treated, the method has the advantages of easy solid-liquid separation, good recycling performance and no secondary pollution.
3. According to the invention, the prepared aluminum sludge-based spherical uranium adsorbent has high-efficiency adsorption performance and good selectivity on uranium by treating low-concentration uranium-containing wastewater.
The detailed structure of the present invention will be further described with reference to the accompanying drawings and the detailed description.
Drawings
FIG. 1 is an electron microscope scanning image of aluminum sludge powder;
FIG. 2 is an electron microscope scan of a prepared non-freeze dried uranium adsorption gel sphere;
FIG. 3 is an electron microscope scanning image of the prepared uranium adsorption gel spheres;
FIG. 4 is a graph showing the influence of uranium-containing wastewater with different uranium concentrations on the removal rate;
FIG. 5 is a graph showing the influence of pH value uranium-containing wastewater on the removal rate;
FIG. 6 is a graph showing the influence of uranium-containing wastewater on the removal rate in the uranium adsorption gel ball dosage amount of different aluminum sludge;
FIG. 7 is a graph showing the influence of uranium-containing wastewater of different oscillation reaction times on the removal rate;
FIG. 8 is a bar graph of the effect of uranium-containing wastewater with different interfering ions on removal rate;
FIG. 9 is an electron microscope scan of uranium adsorbing gel spheres of uranium adsorbed aluminum sludge;
fig. 10 is a graph of uranium removal rate of three times of recycling of uranium-adsorbing gel spheres of aluminum sludge.
Detailed Description
Example one, the preparation of uranium adsorption gel balls based on aluminum sludge includes the following steps,
A. pretreatment of aluminum sludge
Taking the aluminum sludge obtained after water purification in a water plant, washing surface impurities of the aluminum sludge by deionized water, then placing the aluminum sludge in a blast drying oven at 100 ℃ for 8 hours, grinding and crushing the dried aluminum sludge to obtain aluminum sludge powder, sieving the aluminum sludge powder by a 100-mesh sieve, and sealing and storing the aluminum sludge powder for later use.
The aluminum sludge is obtained from a water plant, and the flocculating agent used for purifying the water body is polyaluminium chloride iron. In the aluminum sludge, aluminum and iron exist in the form of oxides, and the percentage content of main elements is as follows:
element(s) | C | O | Mg | Al | Si | S | Cl | K | Ca | Fe |
Percentage content (%) | 26.26 | 43.25 | 1.52 | 6.27 | 9.86 | 1.53 | 1.30 | 1.44 | 3.45 | 5.12 |
B. Preparation of the aqueous Sol solution
Dissolving polyvinyl alcohol in distilled water, heating and magnetically stirring until the polyvinyl alcohol is completely dissolved, cooling, sequentially adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring until the mixture is uniformly mixed; wherein, the weight ratio of polyvinyl alcohol: aluminum sludge powder: the mass fraction ratio of the sodium alginate is 1: 1.5: 0.5.
C. preparation of uranium adsorption gel balls
After the mixture is magnetically stirred, the mixture is in a sticky state according to the ratio of the mixture to CaCl2The mass ratio of the solution is 1: 10, 3 percent of CaCl by mass fraction2Injecting and extruding the solution, dripping the solution into the mixture, and curing for 30min until the mixture is in a gel ball shape;
D. drying of uranium adsorbed gel spheres
Washing the gel-ball mixture with deionized water and anhydrous ethanol for several times until the solution is neutral, and removing CaCl on the surface2And then placing the mixture in a vacuum freeze dryer at the temperature of 20 ℃ below zero for drying for 12 hours to prepare the uranium adsorption gel balls.
Example two, the preparation of uranium adsorption gel balls based on aluminum sludge comprises the following steps,
A. pretreatment of aluminum sludge
Taking the aluminum sludge obtained after water purification in a water plant, washing surface impurities of the aluminum sludge by deionized water, then placing the aluminum sludge in a forced air drying oven at 130 ℃ for 7h, grinding and crushing the dried aluminum sludge to obtain aluminum sludge powder, sieving the aluminum sludge powder by a 100-mesh sieve, and sealing and storing the aluminum sludge powder for later use.
The aluminum sludge is obtained from a water plant, and the flocculating agent used for purifying the water body is polyaluminium chloride iron. In the aluminum sludge, aluminum and iron exist in the form of oxides, and the percentage content of main elements is as follows:
element(s) | C | O | Mg | Al | Si | S | Cl | K | Ca | Fe |
Percentage content (%) | 26.26 | 43.25 | 1.52 | 6.27 | 9.86 | 1.53 | 1.30 | 1.44 | 3.45 | 5.12 |
B. Preparation of the aqueous Sol solution
Dissolving polyvinyl alcohol in distilled water, heating and magnetically stirring until the polyvinyl alcohol is completely dissolved, cooling, sequentially adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring until the mixture is uniformly mixed; wherein, the weight ratio of polyvinyl alcohol: aluminum sludge powder: the mass fraction ratio of the sodium alginate is 1: 2: 0.7.
C. preparation of uranium adsorption gel balls
After the mixture is magnetically stirred, the mixture is in a sticky state according to the ratio of the mixture to CaCl2The mass ratio of the solution is 1: 20, 3 percent of CaCl by mass fraction2The solution is injected and extruded into the mixture and cured for 40min to obtain the spherical gel.
D. Drying of uranium adsorbed gel spheres
Washing the gel-ball mixture with deionized water and anhydrous ethanol for several times until the solution is neutral, and removing CaCl on the surface2And then placing the mixture in a vacuum freeze dryer at the temperature of 20 ℃ below zero for drying for 12 hours to prepare the uranium adsorption gel balls.
Example three, the preparation of uranium adsorption gel balls based on aluminum sludge includes the following steps,
A. pretreatment of aluminum sludge
Taking aluminum sludge obtained after water body purification in a water plant, washing surface impurities of the aluminum sludge by deionized water, then placing the aluminum sludge in a forced air drying oven at 150 ℃ for 6 hours, grinding and crushing the dried aluminum sludge to obtain aluminum sludge powder, sieving the aluminum sludge powder by a 100-mesh sieve, and sealing and storing the aluminum sludge powder for later use;
the aluminum sludge is obtained from a water plant, and the flocculating agent used for purifying the water body is polyaluminium chloride iron. In the aluminum sludge, aluminum and iron exist in the form of oxides, and the percentage content of main elements is as follows:
element(s) | C | O | Mg | Al | Si | S | Cl | K | Ca | Fe |
Percentage content (%) | 26.26 | 43.25 | 1.52 | 6.27 | 9.86 | 1.53 | 1.30 | 1.44 | 3.45 | 5.12 |
B. Preparation of the aqueous Sol solution
Dissolving polyvinyl alcohol in distilled water, heating and magnetically stirring until the polyvinyl alcohol is completely dissolved, cooling, sequentially adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring until the mixture is uniformly mixed; wherein, the weight ratio of polyvinyl alcohol: aluminum sludge powder: the mass fraction ratio of the sodium alginate is 1: 3: 1;
C. preparation of uranium adsorption gel balls
After the mixture is magnetically stirred, the mixture is in a sticky state according to the ratio of the mixture to CaCl2The mass ratio of the solution is 1: 30, 3 percent of CaCl by mass fraction2Injecting and extruding the solution and dripping the solution into the mixture, and curing for 45min until the mixture is in a gel ball shape to obtain a uranium adsorption gel ball;
D. drying of uranium adsorbed gel spheres
Washing the gel-ball mixture with deionized water and anhydrous ethanol for several times until the solution is neutral, and removing CaCl on the surface2Then placing the mixture in a vacuum freeze dryer at the temperature of-20 ℃ for drying for 12 hours.
And (3) respectively observing the aluminum sludge powder pretreated in the step (A), the unfrozen uranium adsorption gel balls prepared in the step (C) and the uranium adsorption gel balls dried in the step (D) by adopting electron microscope scanning, specifically adopting JSM-7500F field emission electron microscope Scanning (SEM) under the instrument setting condition of WD22mm Spotsize20, placing the prepared uranium adsorption gel on a sample seat, plating a conductive film, and observing the uranium adsorption gel, wherein the observation results are respectively shown in figures 1-3. As shown in FIG. 1, the material surface of the aluminum sludge powder is mostly of a layered structure, and the aperture is large; as shown in figure 2, the prepared uranium adsorption gel balls which are not frozen and dried are spherical, and the particle size is 2.9-3.1 mm; it is seen from fig. 3 that the material pore diameter of the dried uranium adsorption gel spheres becomes smaller, and fig. 1-3 illustrate that polyvinyl alcohol and sodium alginate in the dried uranium adsorption gel spheres are well attached to the surface of the aluminum sludge powder.
Example four, the method for treating uranium-containing wastewater by using uranium adsorption gel balls based on aluminum sludge, wherein the concentration of uranium in the uranium-containing wastewater is 2 mg/L-25 mg/L, and the pH value is 2-8, comprises the following steps,
adjusting the pH value of the uranium-containing wastewater to 2-7, then adding uranium adsorption gel balls based on aluminum sludge according to the addition amount of 0.4-0.8 g/L, wherein the adsorption adopts a constant-temperature shaking table to oscillate and react for 0.5-6 h, the constant-temperature adsorption temperature is 15-35 ℃, and the oscillation frequency of the constant-temperature shaking table is 160 r/min.
Detecting the concentration of residual uranium in the uranium-containing wastewater by adopting an ultraviolet-spectrophotometry to the removal rate of the uranium-containing wastewater, and calculating the removal rate and removal capacity of uranium adsorption gel balls of aluminum sludge to the uranium-containing wastewater according to the following formula:
wherein Q iseThe removing rate of uranium solution by uranium adsorption gel balls of aluminum sludge is percent; r is the adsorption capacity of uranium adsorption gel balls of the aluminum sludge to uranium, and the unit is mg/g; c0The initial concentration of uranium in the uranium-containing wastewater is mg/L; c is the residual concentration of uranium in the uranium-containing wastewater after being treated by uranium adsorption gel balls of aluminum sludge, and the unit is mg/L; v is the volume of the solution, and the unit is L; m is the mass of the uranium adsorption gel balls of the aluminum sludge, and the unit is mg.
The removal rate and the removal capacity of uranium-bearing wastewater treated by uranium adsorption gel balls of aluminum sludge under different conditions are analyzed, and the results are as follows:
the method comprises the following steps of (I) carrying out adsorption detection on uranium-containing wastewater with different uranium concentrations: adjusting the pH value of the uranium-containing wastewater to 4, then respectively putting uranium adsorption gel balls based on aluminum sludge into the uranium-containing wastewater with uranium concentration of 2mg/L, 5mg/L, 10mg/L, 15mg/L, 20mg/L and 25mg/L according to the addition of 0.6g/L, setting the adsorption reaction time of 4h by adopting constant-temperature shaking table oscillation, setting the constant-temperature adsorption temperature of 25 ℃ and the constant-temperature shaking table oscillation frequency of 160r/min, and calculating the removal rate of uranium in the uranium-containing wastewater with different uranium concentrations. The results showed that the removal rates of uranium were 99.25%, 95.92%, 94.86%, 90.62%, 88.41%, 83.17%, respectively.
Fig. 4 shows a graph of the influence of uranium-containing wastewater with different uranium-containing concentrations on the removal rate and the removal capacity, and it is seen from fig. 4 that the removal rate is always reduced along with the increase of the uranium concentration in the uranium-containing wastewater, and the removal rate reaches more than 94% within the range of 2-10 mg/L of the uranium-containing concentration in a normal temperature system.
(II) carrying out adsorption detection on the uranium-containing wastewater with different pH values: the concentration of uranium is 10mg/L in the uranium-bearing waste water, adjust the pH value of uranium-bearing waste water to 2 respectively, 3, 4, 5, 6, 7, then according to 0.6 g/L's addition will be based on the uranium adsorption gel ball of aluminium mud drops into the uranium-bearing waste water, it adopts constant temperature shaking table oscillation reaction time to be 4h to set up the adsorption reaction, constant temperature adsorption temperature is 25 ℃, the frequency of constant temperature shaking table oscillation is 160r/min, calculate the clearance and the removal capacity of uranium in the uranium-bearing waste water of different uranium-bearing concentrations. The results showed that the removal rates of uranium were 17.89%, 75.45%, 95.03%, 92.11%, 77.16%, 31.98%, respectively.
FIG. 5 shows a graph of the influence of uranium-containing wastewater with different pH values on the removal rate and the removal capacity, and it can be seen from FIG. 5 that the removal rate and the removal capacity show an ascending trend in the pH adjustment range of 2-4, reach a maximum value when the pH is adjusted to 4, and then start to gradually decline.
(III) adsorbing and detecting the uranium-containing wastewater with the uranium adsorption gel ball adding amount of different aluminum sludge: the concentration of uranium in the uranium-containing wastewater is 10mg/L, adjust the pH value of the uranium-containing wastewater to 4, then respectively according to the addition of 0.4g/L, 0.5g/L, 0.6g/L, 0.7g/L, 0.8g/L put uranium adsorption gel balls based on aluminum sludge into the uranium-containing wastewater, set the adsorption reaction to adopt constant temperature shaking table oscillation reaction time to be 4h, the constant temperature adsorption temperature is 25 ℃, the frequency of constant temperature shaking table oscillation is 160r/min, calculate the removal rate and removal capacity of uranium in the uranium-containing wastewater with different uranium-containing concentrations. The results show that the uranium removal rates are 85.58%, 90.45%, 95.03%, 95.21%, 94.86, respectively.
Fig. 6 shows a graph of the influence of uranium-bearing wastewater of uranium adsorption gel ball dosage of different aluminum sludge on the removal rate and the removal capacity, and it is seen from fig. 6 that when the uranium adsorption gel ball dosage of aluminum sludge is 0.4g/L, the uranium removal rate is the largest, but the uranium removal rate is lower, and along with the increase of the uranium adsorption gel ball dosage of aluminum sludge, the uranium removal rate gradually rises to a certain level, and the uranium removal rate gradually decreases. Comprehensively considering, the effect of removing the low-concentration uranium-containing wastewater is the best when the adding amount of the uranium adsorption gel balls of the aluminum sludge is 0.6 g/L.
(IV) carrying out adsorption detection on the uranium-containing wastewater with different oscillation reaction times: the concentration of uranium is 10mg/L in the uranium-containing waste water, adjust the pH value of uranium-containing waste water to 4, then drop into uranium-containing waste water based on the uranium adsorption gel ball of aluminium mud according to 0.6 g/L's addition, it adopts constant temperature shaking table oscillation reaction time to set up the adsorption reaction and is 0.5h respectively, 1h, 1.5h, 2h, 2.5h, 3h, 3.5h, 4h, 5h, 6h, the constant temperature adsorption temperature is 25 ℃, the frequency of constant temperature shaking table oscillation is 160r/min, calculate the clearance of uranium-containing waste water uranium-containing of different uranium-containing concentrations. The results showed that the uranium removal rates were 60.15%, 75.62%, 82.49%, 85.24%, 89.02%, 90.22%, 92.11%, 95.03%, 94.69%, 95.03%, respectively.
Fig. 7 shows a graph of the influence of uranium-containing wastewater of different oscillation reaction times on the removal rate and the removal capacity, and it is seen from fig. 7 that the uranium adsorption gel balls of aluminum sludge substantially go through three stages to remove uranium-containing wastewater, the removal capacity is in a rapidly rising state within 0-1 h, the removal capacity is in a slowly rising state within 1-4 h, and gradually reaches an equilibrium state after 4h, so that the oscillation reaction time of the uranium adsorption gel balls of aluminum sludge to remove uranium-containing wastewater is more than 4h, and the effect is optimal.
(V) adsorb the detection to the uranium-bearing waste water that has different interference ions, because probably only contain uranium in the actual uranium-bearing waste water, other interference impurity such as copper, calcium, chloridion in addition, for the adsorption effect of further observation aluminium sludge's uranium adsorption gel ball to uranium, detect uranium removal rate and removal capacity under the condition that has different interference ions in the uranium-bearing waste water. The method specifically comprises the following steps: the concentration of uranium in the uranium-bearing waste water is 10mg/L, adjusts the pH value of uranium-bearing waste water to 4, then according to 0.6 g/L's addition will be based on the uranium adsorption gel ball of aluminium mud and drop into the uranium-bearing waste water, according to uranium and interference ion 1 in the uranium-bearing waste water: 1 ratio of Cu to be added2+、Ca2+、Pb2+、SO4 2-、Cl-、NO3 -And as interference ions, setting the oscillation reaction time of a constant-temperature shaking table for the adsorption reaction to be 4h respectively, setting the constant-temperature adsorption temperature to be 25 ℃, setting the oscillation frequency of the constant-temperature shaking table to be 160r/min, and calculating the removal rate of uranium in uranium-containing wastewater with different uranium concentration. The results showed that the uranium removal rates were 90.40%, 92.97%, 94.52%, 94.00%, 94.35%, 94.69%, respectively.
FIG. 8 shows a bar graph of the effect of uranium-containing wastewater in the presence of different interfering ions on removal rate, as seen in FIG. 8The uranium adsorption gel ball that goes out aluminium mud all reaches more than 90% to the clearance of uranium, and the uranium adsorption gel ball of aluminium mud has good selectivity to uranium, and the interference ion is the cation to the influence degree that uranium adsorption gel ball of aluminium mud got rid of uranium-bearing waste water: cu2+>Ca2+>Pb2+The anion: SO (SO)4 2->Cl->NO3 -。
The uranium adsorption gel balls adsorbing the uranium-bearing aluminum sludge are observed by adopting electron microscope scanning, specifically JSM-7500F field emission electron microscope Scanning (SEM), the setting condition of the instrument is WD22mm Spotsize20, the uranium adsorption gel balls adsorbing the uranium-bearing aluminum sludge are placed on a sample seat, the uranium adsorption gel balls are observed after being plated with a conductive film, the observation result is shown in figure 9, the situation that the surface of the uranium adsorption gel balls adsorbing the uranium-bearing aluminum sludge is smooth and has a plurality of protrusions is seen from figure 9, and therefore the uranyl ions in the uranium-bearing wastewater are adsorbed by the uranium adsorption gel balls adsorbing the aluminum sludge.
Separating the saturated uranium adsorption gel spheres from the uranium-containing wastewater after the uranium adsorption gel spheres of the aluminum sludge are adsorbed and saturated, putting the uranium adsorption gel spheres into hydrochloric acid or nitric acid for desorption, then placing a hydrochloric acid or nitric acid solution containing the saturated uranium adsorption gel spheres of the aluminum sludge in a constant-temperature oscillation box for oscillation for 4-6 h, wherein the constant-temperature oscillation temperature is 15-35 ℃, filtering and washing the oscillated solution to be neutral, drying and recycling the uranium adsorption gel spheres of the desorbed aluminum sludge for three times, and detecting and calculating the uranium removal rate of the uranium adsorption gel spheres of the aluminum sludge at each time. Fig. 10 shows the uranium removal rate after the uranium adsorption gel balls of the aluminum sludge are recycled for three times, and it is seen from fig. 10 that the uranium removal rate is still more than 92% after the uranium adsorption gel balls of the aluminum sludge are recycled for three times, so that the uranium adsorption gel balls of the aluminum sludge can remove uranium in uranium-containing wastewater for many times, and the uranium adsorption gel balls have good recycling performance.
Claims (2)
1. The preparation of uranium adsorption gel balls based on aluminum sludge is characterized in that: comprises the following steps of (a) carrying out,
A. pretreatment of aluminum sludge
Taking aluminum sludge obtained after water purification in a water plant, washing surface impurities of the aluminum sludge by deionized water, then placing the aluminum sludge in a forced air drying oven at 100-150 ℃ for 6-8 h, grinding and crushing the dried aluminum sludge to obtain aluminum sludge powder, sieving the aluminum sludge powder by a 100-mesh sieve, and sealing and storing the aluminum sludge powder for later use;
B. preparation of the aqueous Sol solution
Dissolving polyvinyl alcohol in distilled water, heating and magnetically stirring until the polyvinyl alcohol is completely dissolved, cooling, sequentially adding aluminum sludge powder and sodium alginate into the solution, and magnetically stirring until the mixture is uniformly mixed; wherein, the weight ratio of polyvinyl alcohol: aluminum sludge powder: the mass fraction ratio of the sodium alginate is 1: 1.5-3: 0.5 to 1;
C. preparation of uranium adsorption gel balls
After the mixture is magnetically stirred, the mixture is in a sticky state according to the ratio of the mixture to CaCl2The mass ratio of the solution is 1: 10-30 percent of CaCl with the mass fraction of 3 percent2Injecting and extruding the solution and dripping the solution into the mixture, and curing for 30-45 min until the mixture is in a gel ball shape;
D. drying of uranium adsorbed gel spheres
Washing the gel-ball mixture with deionized water and anhydrous ethanol for several times until the solution is neutral, and removing CaCl on the surface2And then placing the mixture in a vacuum freeze dryer at the temperature of 20 ℃ below zero for drying for 12 hours to prepare the uranium adsorption gel balls.
2. The method for treating uranium-bearing wastewater by using uranium adsorption gel balls based on aluminum sludge as claimed in claim 1, wherein the concentration of uranium in the uranium-bearing wastewater is 2-25 mg/L, and the pH value is 2-8, and the method is characterized in that: comprises the following steps of (a) carrying out,
adjusting the pH value of the uranium-containing wastewater to 4-6, then adding uranium adsorption gel balls based on aluminum sludge according to the addition amount of 0.4-0.8 g/L, wherein the adsorption adopts a constant-temperature shaking table to oscillate and react for 0.5-6 h, the constant-temperature adsorption temperature is 15-35 ℃, and the oscillation frequency of the constant-temperature shaking table is 160 r/min.
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