CN107913665B - Metal-doped boehmite as well as preparation method and application thereof - Google Patents
Metal-doped boehmite as well as preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of material synthesis, and particularly relates to metal-doped boehmite as well as a preparation method and application thereof. The method takes double metal salt as a raw material, uses metal doped ions in a certain proportion, adopts sodium citrate as a metal complexing agent, and reacts in a mixed solvent with the proportion of water to absolute ethyl alcohol of 1:0.5-2 at the temperature of 220 ℃ for 12-48h to obtain the boehmite doped materials with different morphologies. The invention obtains the doped boehmite with high-efficiency and rapid defluorination by a one-step mixed solvent thermal bimetal doping mode. The method has the advantages of simplicity, convenience, practicability, short flow and the like, and provides a simple and feasible synthesis idea for exploring the synthesis of efficient doped materials.
Description
The technical field is as follows:
the invention belongs to the technical field of adsorption materials, and relates to high-efficiency and rapid defluorination doped boehmite as well as a preparation method and application thereof.
Background art:
in recent years, people's life and industrial production all produce fluoride-containing waste water, such as excessive fluoride solution in toothpaste, and electrolytic zinc in nonferrous metallurgy is easy to produce fluoride ion solution and enrich fluoride ion solution waste water with high concentration of over 1000 ppm. The common wastewater defluorination methods at home and abroad include chemical precipitation, ion exchange, membrane filtration, adsorption, electrocoagulation and the like. In the case of a fluorine-containing solution having a high concentration, a chemical precipitation method and an adsorption method are mainly used, and since a large amount of calcium oxide is consumed by the chemical precipitation method and the pH of the solution is greatly limited, a large amount of precipitates are generated and are difficult to handle. Adsorption is therefore a better choice and the development of adsorbents for high concentrations of fluoride ion remains an unsolved challenge.
The adsorbents mainly used for adsorbing fluorine ions at present mainly comprise commercial alumina and carbon materials. The general commercial fluoride ion adsorbent has the defects of small adsorption capacity (7.41 mg/g of activated alumina and 23.9mg/g of activated carbon), less hydroxyl groups with adsorption dominance, 8-12h basically needed for reaching saturated adsorption capacity and too low adsorption rate. Although many studies are focused on increasing the adsorption capacity and increasing the adsorption rate, due to the problems of too small specific surface area and too low adsorption group site in the existing fluoride ion adsorbent, Sankhakarmakara et al obtain the metal organic framework of aluminum fumarate as the largest theoretical amount of adsorbed fluorine material by synthetic selection, and the theoretical capacity is 600mg/g at most. Therefore, the adsorption capacity is still difficult to adsorb the high-concentration more than 1000ppm, and the adsorption speed needs to be improved. At present, the defect that the main post-load synthesis mode has a long process is overcome by directly and controllably assembling the loaded solvothermal bimetal doping mode, and the product with the thickness of 300m is obtained2The composite material has large specific surface area and multiple hydroxyl binding sites, and reinforced doped metal sites are introduced, so the composite material has good application prospect in the field of synthesis of adsorption materials.
The invention content is as follows:
the invention aims to provide a series of methods for synthesizing boehmite doped with a high-efficiency and rapid defluorination adsorbent according to the defects of the existing synthetic fluoride ion adsorbent. The method obtains series of doped boehmite by a proper doping mode to obtain series of defluorination adsorbents.
The invention is realized by the following modes:
a preparation method of metal-doped boehmite comprises the steps of mixing a doped metal salt solution and an aluminum salt solution in a certain proportion as precursors, complexing by using a metal complexing agent, and carrying out solvothermal reaction in a reaction kettle for a certain time to obtain the metal-doped boehmite with different morphologies.
The doped metal salt is one of nitrate, sulfate or chloride, and the aluminum salt comprises one or more of aluminum nitrate, aluminum chloride and aluminum sulfate.
The metal ions of the doped metal salt are Mn, Sr, Zr, Ca, Ti, Mg, Fe, Nd, Ce or L a metal ions, wherein the preferred doping element is L a metal salt, and one doped metal salt is preferred for doping.
The molar ratio of the doped metal ions to the Al ions is as follows: 1: 2-16, wherein the most preferred ratio is 1: 3-5.
The metal complexing agent is sodium citrate. Other commonly used complexing agents are tried, and the effect is good without sodium citrate.
The solvent of the solvent heat is a mixed solvent of water and absolute ethyl alcohol in a volume ratio of 1:0.5-2, wherein the most preferable volume ratio is 1: 1.
The sodium citrate: metal salt: the molar ratio of the solvent is 1:2-6:3000-6000, wherein the most preferable ratio is 1:3-5: 3800-4200.
The reaction temperature is 160-220 ℃, and the most preferable temperature is 220 ℃; the reaction time is 12-48h, and the most preferable time is 24 h.
According to the invention, metal-doped boehmite with different morphologies can be obtained according to different doped metal ions.
For example: accurately weighing 1.6mmol Al (NO)3)3·9H2Dissolving O and 0.4mmol lanthanum nitrate in 20m L deionized water and 20m L ethanol, adding 0.5mmol sodium citrate after complete dissolution, ultrasonically oscillating until complete dissolution, transferring to a hydrothermal reaction kettle, reacting for 24h at 220 ℃, cooling to room temperature after complete reaction, taking out the product, repeatedly washing with deionized water and absolute ethanol for several times, and finally drying in an electrothermal constant-temperature air-blowing drying oven at 60 ℃ for 12h to obtain the finished productObtaining the hollow nano-particles.
According to the method, the hollow nano-particles, namely the cerium-doped boehmite material can be obtained only by changing the cerium nitrate hexahydrate with the doping metal of 0.4 mmol.
According to the method, spherical nano particles, namely the neodymium-doped boehmite material can be obtained only by changing the doping metal to be 0.4mmol of neodymium nitrate.
According to the method, spherical nanoparticles, namely the zirconium-doped boehmite material can be obtained only by changing the zirconium chloride with the doping metal of 0.4 mmol.
According to the method, the fried egg type nano particles, namely the iron-doped boehmite material, can be obtained only by changing the iron nitrate nonahydrate doped with 0.4mmol of metal.
According to the method, the fried egg type nano particles, namely the calcium-doped boehmite material can be obtained only by changing the metal-doped anhydrous calcium chloride to be 0.4 mmol.
According to the method, spherical nano particles, namely the magnesium-doped boehmite material can be obtained only by changing magnesium sulfate heptahydrate with the doping metal of 0.4 mmol.
According to the method, spherical nano particles, namely the titanium-doped boehmite material can be obtained only by changing the titanium sulfate with the doping metal of 0.4 mmol.
According to the method, the fried egg type nano particles, namely the strontium-doped boehmite material, can be obtained only by changing the doped metal to be 0.4mmol of strontium nitrate.
According to the method, the hollow nano-particles, namely the manganese-doped boehmite material can be obtained only by changing the doped metal to be 0.4mmol of manganese nitrate.
The method is characterized in that metal-doped boehmite is used as an adsorbent, fluoride ion wastewater is treated, the adsorbent is added into fluoride-containing wastewater at the ratio of 1 g/L for adsorption for 30min, wherein the concentration of fluoride ions in the fluoride ion wastewater is not more than 2000 mg/L, and the pH value is 2.
The adsorbent prepared by the method has the advantages that:
1. both the adsorbent boehmite and boehmite doped with other elements have better adsorption capacity. Has good selectivity for fluorine ion adsorption and is less influenced by other anions.
2. The preparation of the material which generates yolk-type boehmite and has a hollow morphology is realized by controlling the conditions to achieve the kirkendall effect, so that a boehmite structure with better specific surface area and more fluoride ion adsorption interfaces are realized.
3. The adsorption rate of the adsorbent is accelerated by doping, for example, lanthanum-doped boehmite can rapidly exert 80-90% of adsorption performance within 30min, and is beneficial to the adsorption application of the flowing fluoride ion waste liquid.
4. In the experiment, water is used for replacing part of organic solvent as synthetic solvent, so that the synthetic cost is reduced, the recycling is convenient, metal salts with various proportions are directly doped in the synthetic process, and the synthetic process is simpler and more convenient.
Drawings
FIG. 1 is an X-ray powder diffraction (XRD) pattern of examples 1-10 of the present invention.
FIG. 2 is a Scanning Electron Microscope (SEM) image of examples 1-10 of the present invention.
FIG. 3 is a photograph of infrared spectra (IR) of examples 1-10 of the present invention.
FIG. 4 is a graph of the defluorination (at 100 ppm) performance of examples 1-10 of the present invention.
FIG. 5 is a graph of the performance of doping for defluorination (at 100 ppm) at different ratios L a according to example 1 of the present invention.
FIG. 6 is a transmission electron micrograph of L a doped according to example 1 of the present invention.
FIG. 7 is a graph of the doping defluorination kinetics of L a in example 1 of the present invention.
Fig. 8 is a Ce-doped transmission electron microscope picture of example 2 of the present invention.
Detailed Description
The invention is further illustrated by, but is not limited to, the following examples.
Example 1
Accurately weighing a certain mole number of Al (NO)3)3·9H2O and lanthanum nitrate (as shown in the following table) in various proportionsAdding 0.5mmol of sodium citrate into 20m L deionized water and 20m L ethanol after complete dissolution, carrying out ultrasonic oscillation until complete dissolution, transferring the mixture into a hydrothermal reaction kettle, reacting at 220 ℃ for 24h, cooling to room temperature after complete reaction, taking out a product, repeatedly washing the product by deionized water and absolute ethanol for several times, and finally drying the product in an electrothermal constant-temperature air-blowing drying box at 60 ℃ for 12h to obtain hollow nanoparticles, wherein L a-1, L a-2, L a-3 and L a-4 materials are added according to the raw material proportion in the following table, the adding concentration is 1 g/L, the adsorption time is 30min, and the adsorption effect of the fluoride ion wastewater (the fluoride ion concentration is 100 mg/L and the pH is 7) is 45.2mg/g, 50.1mg/g, 43.8mg/g and 43.6mg/g respectively.
Example 2
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to be 0.4mmol of cerium nitrate hexahydrate to obtain the hollow nano-particles, namely the cerium-doped boehmite material.
Example 3
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doping metal to be neodymium nitrate with 0.4mmol, so as to obtain spherical nano particles, namely the neodymium-doped boehmite material.
Example 4
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to be zirconium chloride of 0.4mmol, so as to obtain spherical nano particles, namely the zirconium-doped boehmite material.
Example 5
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to 0.4mmol ferric nitrate nonahydrate to obtain omelette-type nanoparticles, namely the iron-doped boehmite material.
Example 6
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to 0.4mmol of anhydrous calcium chloride to obtain the omelette-type nano particles, namely the calcium-doped boehmite material.
Example 7
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doping metal to 0.4mmol of magnesium sulfate heptahydrate to obtain spherical nano particles, namely the magnesium-doped boehmite material.
Example 8
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to 0.4mmol titanium sulfate to obtain spherical nano particles, namely the titanium-doped boehmite material.
Example 9
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doped metal to be strontium nitrate of 0.4mmol, thus obtaining the omelette-type nano-particles, namely the strontium-doped boehmite material.
Example 10
By the method of example 1, Al (NO)3)3·9H2O1.6 mmol, and changing the doping metal to be 0.4mmol of manganese nitrate to obtain the hollow nano-particles, namely the manganese-doped boehmite material.
Example 11
Using the adsorbent materials of examples 1-10, fluorine-containing wastewater was added at 1 g/L for 12h of adsorption, and comparative defluorination studies were conducted:
l a-2 lanthanum-doped boehmite was treated with fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, pH 2) and the fluoride ion adsorption amount was 84.75mg/g in example 1, wherein fluoride ion wastewater was adsorbed at a large capacity (wherein the fluoride ion concentration in the fluoride ion wastewater was 2000 mg/L, pH 2), and the fluoride ion adsorption amount was 1275mg/g, and a study of adsorption kinetics was made on fluoride ion adsorption, showing that adsorption capacity of 65% or more was reached at 30s, and adsorption equilibrium of 80-90% was reached at 30 min.
The cerium-doped boehmite is used for treating fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater is 100 mg/L, and the pH value is 2), and the adsorption amount of the fluoride ion is 83.875 mg/g.
Neodymium-doped boehmite was treated with fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, pH 2) and the adsorption amount of fluoride ions was 83 mg/g.
The zirconium-doped boehmite was used for treating fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, and the pH was 2), and the adsorption amount of fluoride ions was 83.125 mg/g.
The boehmite doped with iron is used for treating fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater is 100 mg/L, and the pH value is 2), and the adsorption capacity to fluoride ions is 76.625 mg/g.
Calcium-doped boehmite was used to treat fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, pH 2) and the fluoride ion adsorption capacity was 81.875 mg/g.
The magnesium-doped boehmite is used for treating fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater is 100 mg/L, and the pH value is 2), and the adsorption amount of fluoride ions is 79.875 mg/g.
Titanium-doped boehmite was treated with fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, pH 2) and the fluoride ion adsorption amount was 78.625 mg/g.
Strontium-doped boehmite was treated with fluoride ion wastewater (fluoride ion concentration in fluoride ion wastewater was 100 mg/L, pH 2) and fluoride ion adsorption amount was 82 mg/g.
Manganese-doped boehmite was treated with fluoride ion wastewater (wherein the fluoride ion concentration in the fluoride ion wastewater was 100 mg/L, pH 2) and the fluoride ion adsorption amount was 81.375 mg/g.
Claims (9)
1. A preparation method of metal-doped boehmite is characterized by comprising the steps of mixing a doped metal salt solution and an aluminum salt solution in a certain proportion as precursors, complexing by using a metal complexing agent, carrying out solvothermal reaction in a reaction kettle for a certain time to obtain the metal-doped boehmite with different morphologies, wherein metal ions of the doped metal salt are Mn, Sr, Zr, Ca, Ti, Mg, Fe, Nd, Ce or L a metal ions, the molar ratio of the doped metal ions to Al ions is 1: 2-16, the metal complexing agent is sodium citrate, the solvothermal solvent is a mixed solvent with the volume ratio of water to absolute ethyl alcohol of 1:0.5-2, the molar ratio of the sodium citrate to the metal salt to the solvent is 1:2-6:3000-6000, the reaction temperature is 160-.
2. The method according to claim 1, wherein the doping metal salt is one of nitrate, sulfate or chloride, and the aluminum salt comprises one or more of aluminum nitrate, aluminum chloride and aluminum sulfate.
3. The method according to claim 1 or 2, wherein the metal ion of the doped metal salt is L a.
4. The production method according to claim 1 or 2, wherein the molar ratio of the doping metal ion to the Al ion is 1: 3-5.
5. The method according to claim 1, wherein the solvent is a mixed solvent of water and absolute ethanol at a volume ratio of 1: 1.
6. The method of claim 1, wherein the ratio of sodium citrate: metal salt: the molar ratio of the solvent is 1:3-5: 3800-4200.
7. The method of claim 1, wherein the reaction temperature is 220 ℃; the reaction time was 24 h.
8. A metal-doped boehmite produced by the method of any one of claims 1-7.
9. The metal-doped boehmite according to claim 8 for use in defluorination.
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