CN114225895B - La-Fe-Al composite metal oxide, preparation method and application - Google Patents
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Abstract
The invention relates to a La-Fe-Al composite metal oxide, a preparation method and application thereof, wherein the La-Fe-Al composite metal oxide comprises the following components in percentage by volume: LaCl330-35% of solution and FeCl323-30% of solution and AlCl33-12% of solution and 32-37% of citric acid solution, and the LaCl3Solution, FeCl3Solution, AlCl3The solution is prepared from LaCl3•7H2O、FeCl3•6H2O、AlCl3•6H2O and citric acid solid powder are respectively dissolved in deionized water and mixed to obtain the product. The invention adopts the LaFeO prepared by the citric acid sol-gel method3Used for adsorbing phosphate in water body due to formed LaFeO3The crystallinity is high, the structure is stable, La and Fe have saturated coordination numbers and are not beneficial to adsorbing phosphate, therefore, the LaFe is prepared by doping aluminum to replace ironxAl1‑xO3The introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent, and in addition, the introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent due to Al3+The valence state is unchanged, the coordination saturation of La and Fe can be reduced, and the oxygen defect proportion of the material is increased, so that the adsorption performance is improved.
Description
Technical Field
The invention relates to the technical field of adsorption materials, in particular to a La-Fe-Al composite metal oxide, a preparation method and application thereof.
Background
The eutrophication phenomenon of water has become a very serious environmental problem in China and even worldwide, for example, the American Yili lake has undergone a great amount of eutrophication events in the past half or more century, so that the aquatic ecosystem is seriously damaged, and large-scale algae outbreaks caused by eutrophication in the Chinese Taihu lake basin directly cause economic losses of $ 65 hundred million. Wherein, phosphorus is considered as a limiting factor causing water eutrophication, and the water eutrophication process is accelerated when the phosphorus concentration in the water exceeds 0.02mg/L, so that how to remove phosphorus elements in the water is of great significance.
The existing phosphorus removal method mainly comprises a biological method, a chemical precipitation method, an adsorption method and the like. Biological phosphorus removal has been applied to a plurality of countries, but microorganisms are sensitive to water quality change conditions, especially temperature and pH value, and aiming at low-concentration phosphorus-containing wastewater, microorganism metabolism is weakened, and phosphorus removal efficiency is very low. The chemical precipitation method can generally reduce the phosphorus concentration to 0.5-1.0 mg/L, and when the phosphorus concentration is reduced to below 0.5mg/L, a large amount of medicament needs to be added, so that the sludge yield and the treatment cost are rapidly increased. The adsorption method is considered to be a feasible phosphorus removal method due to the advantages of low cost, simple operation, environmental friendliness and high removal rate, but the core of the method lies in the development of excellent adsorption materials.
The perovskite oxide can be applied to the adsorption of phosphorus, and the chemical formula of the perovskite oxide is ABO3(A-rare earth elements, e.g. La, Nd, Sm; B-transition metals, e.g. Fe, Mn, Co, Al, Cr) when the cation radius rA>0.90Å，rB>At 0.51A, typically the A site atoms are located at the center of the body and coordinated with 12O's and the B atoms are located at the vertices and coordinated with 6O's to form octahedral structures with coterminous connections between the octahedra through oxygen, so many metal cations are at the perovskite ABO3Stable performance is shown in the structure. This also results in many metal cations, although having a better affinity for oxoanions (e.g., phosphates), still exhibiting poor adsorption capabilities. In view of the above, how to develop an excellent adsorbent for improving the phosphate adsorption capacity is an urgent technical problem to be solved in the art.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide an La-Fe-Al composite metal oxide, a preparation method and application, wherein the La-Fe-Al composite metal oxide is prepared by doping aluminum to replace ironxAl1-xO3The introduction of aluminum can improve the isoelectric point and the specific surface area of the adsorbent and increase the oxygen defect ratio of the material, thereby improvingHigh adsorption performance.
The invention is realized by the following technical scheme:
a La-Fe-Al composite metal oxide comprises the following components in percentage by volume: LaCl330-35% of solution and FeCl323-30% of solution and AlCl33-12% of solution and 32-37% of citric acid solution, and the LaCl3Solution, FeCl3Solution, AlCl3The solution is prepared from LaCl3•7H2O、FeCl3•6H2O、AlCl3•6H2O and citric acid solid powder are respectively dissolved in deionized water and mixed to obtain the product.
According to the above technical solution, preferably, the LaCl is3Solution, FeCl3Solution, AlCl3The concentration of the solution is 0.2mol/L, and the concentration of the citric acid solution is 1 mol/L.
According to the above technical solution, preferably, the following components are included by volume: LaCl3Solution 33% FeCl328-30% of solution and AlCl33-5% of solution and 34% of citric acid solution.
According to the technical scheme, the additive preferably comprises the following components in percentage by volume: LaCl3Solution 33% FeCl323-25% of solution and AlCl310-12% of solution and 32% of citric acid solution.
The invention also discloses a preparation method of the La-Fe-Al composite metal oxide, which comprises the following steps: a. respectively preparing 0.2mol/L of LaCl3Solution, FeCl3Solution, AlCl3Solution and 1mol/L citric acid solution; b. the LaCl is added according to the volume ratio3Solution, FeCl3Solution, AlCl3Mixing the solutions, and dropwise adding a citric acid solution under a stirring state; c. stirring for 1.5-2h, and evaporating for 24-30h in a constant-temperature water bath environment to obtain wet gel; d. drying the wet gel in an oven at the temperature of 110-130 ℃ for 24h to obtain dry gel; e. crushing the dry gel, putting the crushed dry gel into a tube furnace, heating to 400 ℃, roasting for 2h, heating to 800 ℃, roasting for 2h, cooling to room temperature to obtain a red powder solid product LaFexAl1-xO3。
According to the above technical solution, preferably, the water bath temperature in step c is 80 ℃.
According to the above technical solution, preferably, step e includes: the dry gel is crushed and transferred to a crucible and is placed into a tube furnace; opening the seals at two sides of the tube furnace; firstly, heating to 400 ℃ at the heating rate of 5 ℃ per minute, and roasting for 2 hours; then the temperature is increased to 800 ℃ and the mixture is calcined for 2h, and after the mixture is cooled to the room temperature, a red powder solid product LaFe is obtainedxAl1-xO3。
The invention also discloses application of the La-Fe-Al composite metal oxide in adsorbing phosphate, wherein the La-Fe-Al composite metal oxide adsorbs the phosphate under the environment that the pH value is 3-7.
The invention has the beneficial effects that:
the invention adopts the LaFeO prepared by the citric acid sol-gel method3Used for adsorbing phosphate in water body due to the formed LaFeO3The crystallinity is high, the structure is stable, La and Fe have saturated coordination numbers and are not beneficial to adsorbing phosphate, therefore, the LaFe is prepared by doping aluminum to replace ironxAl1-xO3The introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent, and in addition, the introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent due to Al3+The valence state is unchanged, the coordination saturation of La and Fe can be reduced, and the oxygen defect proportion of the material is increased, so that the adsorption performance is improved.
Drawings
FIG. 1 is a schematic diagram of XRD characterization analysis of test group S1, test group S2 and comparative group D in the present invention.
FIG. 2 is a graph showing the comparison of the adsorption amounts of phosphate at different pH levels among the test group S1, the test group S2, and the comparative group D according to the present invention.
Detailed Description
In order to make the technical solutions of the present invention better understood by those skilled in the art, the present invention will be further described in detail with reference to the accompanying drawings and preferred embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
A La-Fe-Al composite metal oxide comprises the following componentsVolume ratio components: LaCl330-35% of solution and FeCl323-30% of solution and AlCl33-12% of solution and 32-37% of citric acid solution, and the LaCl3Solution, FeCl3Solution, AlCl3The solution is prepared from LaCl3•7H2O、FeCl3•6H2O、AlCl3•6H2O and citric acid solid powder are respectively dissolved in deionized water and mixed to obtain the product. Wherein, the LaCl3Solution, FeCl3Solution, AlCl3The concentration of the solution is 0.2mol/L, and the concentration of the citric acid solution is 1 mol/L.
Based on the above examples, the present invention prefers the following two embodiments of volume ratio composition:
embodiment 1: LaCl3Solution 33% FeCl328-30% of solution and AlCl33-5% of solution and 34% of citric acid solution;
embodiment 2: LaCl3Solution 33% FeCl323-25% of solution and AlCl310-12% of solution and 32% of citric acid solution.
LaFeO prepared by citric acid sol-gel method is adopted in the research3The perovskite is used for adsorbing phosphate in water, the citric acid sol-gel method has a plurality of advantages, but the corresponding perovskite structure can be formed only by calcining in air at 700-800 ℃, and LaFeO is formed due to the high calcining temperature and sufficient oxygen contact3The perovskite has high crystallinity and stable structure, and La and Fe have saturated coordination numbers and are not beneficial to adsorbing phosphate. In view of this we prepared LaFe by doping with aluminum instead of ironxAl1-xO3The introduction of aluminum to improve the adsorption performance has the following technical principle:
ion doping or partial substitution can cause valence alternation and oxygen defect, ion doping with different radii can generate different strain, Al3+Ionic radius ratio of Fe3+Small ionic radius, Al3+Ion substituted Fe3+After ions are generated, the inter-lattice ion distance is reduced, the grain size is reduced, namely, compressive strain occurs, and the lattice parameter is reduced; on the other hand, Al3+After doping, the crystal lattice structure is distorted, and the degree of the distortion of the crystal lattice is concentrated along with the dopingThe increase in degree increases and the change in dipole moment increases, resulting in an increase in the polarity of the molecules, the greater the van der waals forces, which, as a major electrostatic attraction for adsorption of phosphate, effectively adsorb phosphate ions and increase the mass transfer kinetics of the material for adsorption of phosphate. LaFeO3The medium oxygen exists mainly in two states, namely lattice oxygen and adsorbed oxygen, the adsorbed oxygen is formed by overflowing the lattice oxygen to form oxygen vacancy in the high-temperature synthesis process and adsorbing oxygen in the air in order to maintain the electrical neutrality of the system, but Fe in the high-temperature process3+May be oxidized into Fe4+In order to maintain charge balance, the overflow of lattice oxygen is limited, the amount of adsorbed oxygen is reduced, and at the moment, the unchanged valence state of aluminum ion is introduced, the aluminum ion is firstly combined with oxygen, and Fe4+Is reduced to Fe3+Even part of Fe3+Is reduced to Fe2+In order to maintain charge balance, the oxygen overflow of the crystal lattice is increased and the content of oxygen vacancies is increased, but the change tendency is opposite when too many aluminum ions are introduced because the charge change degree of the material itself is reduced and the oxygen vacancies are reduced.
The invention also discloses a preparation method of the La-Fe-Al composite metal oxide, which comprises the following steps:
a. accurately weighing a certain amount of LaCl according to a stoichiometric ratio3•7H2O（74.274g）、FeCl3/6H2O（54.06g）、AlCl3•6H2O (48.286 g) and citric acid solid powder (192.12 g) were dissolved in 1L of deionized water to prepare 0.2mol/L of LaCl3、FeCl3、AlCl3Solution and 1mol/L citric acid solution.
b. LaCl is added into the mixture according to the following three volume ratios3Solution, FeCl3Solution, AlCl3Mixing the solutions, and dropwise adding a citric acid solution under stirring:
experimental group S1: 100mL of LaCl was taken out3、90mL FeCl3And 10mL AlCl3The solutions are mixed with each other to form a mixed solution of La-Fe-Al, and 100mL of citric acid solution is dripped into the mixed solution under the condition of vigorous stirring;
experimental group S2: 100mL of LaCl was taken out3、70mL FeCl3And 30mL AlCl3The solutions are mixed with each other to form a mixed solution of La-Fe-Al, and 100mL of citric acid solution is dripped into the mixed solution under the condition of vigorous stirring;
comparative group D: 100mL of LaCl was taken out3、100mL FeCl3Mixing the materials to form a La-Fe mixed solution, and dropwise adding 100mL of citric acid solution into the mixed solution under a violent stirring state;
c. stirring the three groups of mixed solutions for 1.5-2h under a magnetic stirrer, and evaporating for 24-30h in a constant-temperature water bath environment at 80 ℃ to obtain wet gel;
d. drying the wet gel in an oven at the temperature of 110-;
e. crushing the dry gel, transferring the crushed dry gel to a crucible, putting the crucible into a tubular furnace, opening the seals at two sides of the tubular furnace to ensure that sufficient air exists in the furnace, firstly heating to 400 ℃ at the heating rate of 5 ℃ per minute, roasting for 2h to remove organic matters per se, then heating to 800 ℃ to calcine for 2h, cooling to room temperature to obtain red powder solid products LaFe in an experiment group S1, an experiment group S2 and a comparison group D respectively0.9Al0.1O3、LaFe0.7Al0.3O3And LaFeO3。
Wherein, the XRD characterization and analysis of FIG. 1 shows that the doped aluminum is pure LaFeO before and after doping3The perovskite phase shows that Al in the experimental group S1 and the experimental group S2 is successfully doped into LaFeO3In perovskite.
The invention also discloses application of the La-Fe-Al composite metal oxide in adsorbing phosphate, wherein the La-Fe-Al composite metal oxide adsorbs the phosphate under the environment that the pH value is 3-7. Specifically, the adsorption capacity of the test group S1, the test group S2 and the comparative group D for phosphate was verified through experiments in the following manner:
(1) preparing a phosphate solution: 4.39g KH are weighed out2PO4Prepare 1000mg/L phosphorus solution, take 30mL to 1L volumetric flask, dilute to 30mg/L with deionized water.
(2) Adjusting the pH of the solution: the pH of the solution is adjusted to 2-12 with 1mol/L NaOH and 1mol/L HCl.
(3) Weighing: 0.02g of LaFeO was weighed3、LaFe0.9Al0.1O3And LaFe0.7Al0.3O3In a 100ml Erlenmeyer flask.
(4) Adding a solution: 50ml of a phosphorus solution having a pH of 2 to 12 and a concentration of 30mg/L was added to each flask.
(5) Culturing: placing the triangular flask into a constant-temperature shaking incubator with the rotation speed of 180r/min and the temperature of 25 ℃ for culture.
(6) Measurement: and taking out a sample after 24 hours, standing, extracting supernate, filtering the supernate with a 0.45-micrometer filter membrane, and measuring the phosphate concentration at the wavelength of 700nm by adopting an ammonium molybdate spectrophotometry.
As can be seen from fig. 2, the initial pH of the solution has a great influence on the adsorption of phosphate by the three adsorbents of experimental group S1, experimental group S2, and comparative group D. Under the strong acid condition (pH = 2), the three adsorbents are dissolved, and the obvious observation is that the adsorption quantity is low and the adsorption effect is poor; when the pH is =3-4, the adsorption quantity is remarkably improved, and LaFeO3Maximum adsorption (pH = 3) 31.11mg/g, LaFe0.9Al0.1O3And LaFe0.7Al0.3O3The maximum adsorption amounts (pH = 4) were 43.06 and 50.83mg/g, respectively, and it was also observed that the adsorption amount gradually increased with increasing aluminum doping amount, probably because phosphate was preferentially bonded to aluminum under acidic conditions; as the pH increases, the phosphate in solution is predominantly HPO4 2-Form exists, HPO4 2-Has larger adsorption energy, so that the adsorption capacity of the three adsorbents is gradually reduced, but the LaFe0.9Al0.1O3And LaFe0.7Al0.3O3Still better than LaFeO3The qualitative improvement shows that the doped aluminum can cause the change of the physical and chemical properties of the material, and the isoelectric point, the specific surface area and the oxygen defect number of the material are improved; when the pH =7-9, the more doped aluminum content, the gradually decreased adsorption amount, again demonstrating that phosphate bonds preferentially to aluminum under acidic conditions and to lanthanum under neutral and alkaline conditions; however, at pH =10-11, LaFe0.7Al0.3O3Adsorption capacity ratio LaFe0.9Al0.1O3High, still kept around 20mg/g, probably because the oxygen defect number increases with the doping aluminum content, and can compensate OH in the solution-The impact caused by the heat; at pH =12, the adsorption capacity of the three materials is significantly reduced, indicating that OH is present under strongly alkaline conditions-Can occupy the adsorption position on the surface of the adsorbent, and compete with phosphate to be unfavorable for the adsorption process. In conclusion, the La-Fe-Al composite metal oxide has better effect of removing phosphorus element in water body for water quality in acid environment.
The invention adopts the LaFeO prepared by the citric acid sol-gel method3Used for adsorbing phosphate in water body due to formed LaFeO3The crystallinity is high, the structure is stable, La and Fe have saturated coordination numbers and are not beneficial to adsorbing phosphate, therefore, the LaFe is prepared by doping aluminum to replace ironxAl1-xO3The introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent, and in addition, the introduction of aluminum can increase the isoelectric point and specific surface area of the adsorbent due to Al3+The valence state is unchanged, the coordination saturation of La and Fe can be reduced, and the oxygen defect proportion of the material is increased, so that the adsorption performance is improved.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (3)
1. The application of the La-Fe-Al composite metal oxide in adsorbing phosphate is characterized in that the La-Fe-Al composite metal oxide adsorbs phosphate under the environment of pH 3-7, and the preparation method of the La-Fe-Al composite metal oxide comprises the following steps:
a. respectively preparing 0.2mol/L of LaCl3Solution, FeCl3Solution, AlCl3Solution and 1mol/L citric acid solution, the LaCl3Solution, FeCl3Solution, AlCl3The solution and the citric acid solution are prepared from LaCl3•7H2O、FeCl3•6H2O、AlCl3•6H2Dissolving solid powders of O and citric acid respectivelyMixing in deionized water;
b. 100mL of LaCl are respectively taken3Solution, 70mL FeCl3Solution and 30mL AlCl3The solutions are mixed with each other to form a mixed solution of La-Fe-Al, and 100mL of citric acid solution is dripped into the mixed solution under the stirring state;
c. stirring for 1.5-2h, and evaporating for 24-30h in a constant-temperature water bath environment to obtain wet gel;
d. drying the wet gel in an oven at the temperature of 110-130 ℃ for 24h to obtain dry gel;
e. crushing the dry gel, putting the crushed dry gel into a tubular furnace, heating to 400 ℃, roasting for 2h, heating to 800 ℃, roasting for 2h, cooling to room temperature to obtain a red powder solid product LaFe0.7Al0.3O3。
2. The use of La-Fe-Al composite metal oxide for adsorbing phosphate according to claim 1, wherein the water bath temperature in step c is 80 ℃.
3. Use of a La-Fe-Al composite metal oxide for adsorbing phosphate according to claim 1, wherein step e comprises: the dry gel is crushed and transferred to a crucible and is placed into a tube furnace; opening the seals at two sides of the tube furnace; firstly, heating to 400 ℃ at the heating rate of 5 ℃ per minute, and roasting for 2 hours; then the temperature is increased to 800 ℃ and the mixture is calcined for 2h, and after the mixture is cooled to the room temperature, a red powder solid product LaFe is obtained0.7Al0.3O3。
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