CN107469760B - Nano CaTiO3Powder adsorbent and preparation method and application thereof - Google Patents
Nano CaTiO3Powder adsorbent and preparation method and application thereof Download PDFInfo
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- CN107469760B CN107469760B CN201710899520.4A CN201710899520A CN107469760B CN 107469760 B CN107469760 B CN 107469760B CN 201710899520 A CN201710899520 A CN 201710899520A CN 107469760 B CN107469760 B CN 107469760B
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Abstract
The invention relates to nano CaTiO3A powder adsorbent and a preparation method and application thereof, belonging to the technical field of nano material preparation and sewage treatment; the method takes metatitanic acid and calcium hydroxide as raw materials for the first time, and prepares the nano calcium titanate by a hydrothermal synthesis method, wherein the higher the hydrothermal synthesis temperature is, the better the morphology of the formed nano calcium titanate is, and the particle size is 800 nm; when the nano calcium titanate with a perfect crystal structure is selected as an adsorbent to treat the wastewater containing heavy metal ions, the excellent adsorption effect is shown; the preparation process of the nano calcium titanate provided by the invention is simple, the reaction is safe, the energy consumption is low, and the raw material price is low; the nano calcium titanate has high adsorption capacity on heavy metal ions, can effectively adsorb the heavy metal ions in sewage, and has good economic, environmental and social benefits. Has wide application prospect in the aspects of new materials and sewage treatment.
Description
Technical Field
The invention relates to nano CaTiO3A powder adsorbent and a preparation method and application thereof, in particular to a method for preparing nano calcium titanate by using metatitanic acid and calcium hydroxide as raw materials through a hydrothermal synthesis method, and the nano calcium titanate is used as an adsorbent for adsorbing heavy metal ions in an aqueous solution, belonging to the technical field of nano material preparation and sewage treatment.
Technical Field
In the thirties of the nineteenth century, perovskite was discovered and analyzed to have TiO as the main mineral component2And CaO, and contains other various elements. Titanates are widely studied among the solid structures of perovskites, and include calcium titanate, strontium titanate, lead titanate, barium titanate, and the like. Calcium titanate (CaTiO)3) Is a most typical ABO3Perovskite oxide of the type wherein the A site is Ca2+The B site is Ti4+. The crystal structure of the calcium titanate being TiO connected by a common apex6The titanium ion with smaller radius is positioned in TiO and is formed by an octahedral three-dimensional network6The octahedral center, which is usually occupied by the larger radius calcium ion, occupies the TiO6Twelve cavities surrounded by octahedrons.
The calcium titanate has a stable crystal structure, high thermal stability, good chemical stability and good biocompatibility, and has very important significance in the aspects of basic research and practical application. In the field of biomedicine, calcium titanate is coated on the surface of titanium and titanium alloy and implanted into human body, so that the bonding strength of titanium and titanium alloy and human body bone tissue can be increased, and the biological inertia of titanium and titanium alloy implanted into human body can be reduced. The document reports that the surface of titanium and titanium alloy is coated with a hydroxyapatite-calcium titanate composite material, and the composite coating integrates the advantages of hydroxyapatite and calcium titanate, has excellent bone tissue binding capacity, is favorable for the adhesion and growth of osteoblasts, and has the characteristic that titanium base is firmly bound and is not easy to separate; in the aspect of sewage treatment, researches show that the nano calcium titanate powder prepared by the sol-gel method has stronger adsorption capacity on lead and cadmium in sewage; in the field of photocatalysis, calcium titanate is a typical wide bandgap semiconductor, but has the potential of visible light response, the morphology with the best ultraviolet radiation photocatalysis performance can be selected, the band gap is narrowed by doping the A site and the B site, or the photocatalysis performance of the calcium titanate is improved by modifying the calcium titanate with materials such as graphene and the like. In these fields, calcium titanate has the advantages of good biocompatibility and excellent performance over other materials.
At present, there are many methods for preparing nano calcium titanate, such as electrostatic spinning method, template method, sol-gel method, solid phase reaction method, microwave heating method, hydrothermal/solvothermal method; the raw materials mainly comprise calcium nitrate, calcium chloride, tetraisopropyl titanate and the like; the raw material price is high, and the mother liquor has the problem of organic pollutants.
Heavy metal means a density of more than 5kg/m3More specifically, the metal of (1) means a metal having an atomic number of 24 or more in the periodic table of elements. Nowadays, sewage treatment and water quality management are one of the important propositions in human life. Along with urbanizationAnd the development of industrial technology, leading to an increase in the amount of garbage accumulated around the world and an increase in heavy metals in water bodies. Heavy metal pollution is different from other organic compound pollution, and even if the concentration of the heavy metal pollution in the environment is very low, the heavy metal pollution is not easily degraded by the self-purification effect of the environment, but can be continuously accumulated in the environment. Heavy metals can not only destroy cell membranes, affect the functions of enzymes and cells, and damage the structure of DNA, but also can be enriched in human bodies by methods such as digesting food and the like. Once the concentration of heavy metal ingested by people exceeds a certain limit, symptoms of acute poisoning, chronic poisoning and the like of the people can be caused. Heavy metals are very toxic, and only trace heavy metal ions are contained in water, so that the toxicity can be generated. The concentration range of the toxicity generated by heavy metals is 1.0-10.0 mg/L. The existing methods for treating heavy metals mainly comprise physical chemistry, electrochemistry and advanced oxidation processes. The physicochemical process includes membrane filtration, chemical precipitation, ion exchange, ultrafiltration and adsorption. The adsorption method is a method for removing or recovering one or more pollutants in the wastewater and purifying the water by taking porous solid as an adsorbent. The adsorbent has the requirements of strong adsorption capacity, low adsorption equilibrium concentration, stable chemical property, good selectivity, easy regeneration and reuse, low cost, wide source and the like. Therefore, the nano calcium titanate is prepared by adopting cheap metatitanic acid and calcium hydroxide as raw materials and utilizing a hydrothermal synthesis method. The nano calcium titanate is used as an adsorbent, and shows good adsorption performance on heavy metal ions in an aqueous solution.
Disclosure of Invention
The invention aims to provide a nano calcium titanate powder adsorbent, a preparation method thereof and a method for adsorbing heavy metal ions.
The invention firstly provides a nano calcium titanate powder adsorbent, which has a calcium titanate crystal structure and a particle size of between 300 and 800 nm.
The invention also provides a preparation method of the nano calcium titanate powder adsorbent, which is characterized in that the calcium titanate is prepared by a hydrothermal synthesis method by taking metatitanic acid and calcium hydroxide as raw materials and carrying out hydrothermal reaction at the temperature of 120-. Specifically, the adsorbent is prepared by the following method:
placing a certain amount of metatitanic acid raw material in a plastic beaker, adding a certain amount of distilled water, uniformly stirring to obtain metatitanic acid slurry, and dropwise adding a sodium hydroxide solution with a certain concentration to neutrality; dispersing a certain amount of calcium hydroxide in a certain volume of distilled water, adding the calcium hydroxide into the metatitanic acid suspension, continuously stirring, and transferring the calcium hydroxide into a hydrothermal reaction kettle. After the hydrothermal reaction is carried out for a period of time, the reaction product is taken out, is filtered to be neutral by distilled water, is placed in a drying oven for drying, and the prepared nano calcium titanate powder is preserved.
Wherein the mass fraction of metatitanic acid in the metatitanic acid raw material is 36 percent (by TiO)2Meter), and the balance of water. The content of industrial-grade calcium hydroxide is 95 percent. NaOH is a commercial industrial grade product with purity>96％。
Wherein the amount of the metatitanic acid raw material is 55.6g, and the amount of the distilled water is 450 mL.
Wherein the concentration of the sodium hydroxide is 2.5 mol/L.
Wherein said Ca (OH)2In an amount of Ca (OH)2A slurry was prepared at a molar ratio of Ca to Ti of metatitanic acid of 1: 1.
Wherein the hydrothermal reaction temperature is 120-180 ℃, and the hydrothermal reaction time is 10-16 h.
Wherein the drying is drying in a drying oven at 80 ℃.
The invention also provides a treatment method for adsorbing heavy metal ions in wastewater by using the nano calcium titanate powder adsorbent, wherein the nano calcium titanate is used as the adsorbent, the adsorption temperature is 20-50 ℃, and the copper, lead and cadmium heavy metal ions in the wastewater are adsorbed.
The specific embodiment is as follows:
adding the nano calcium titanate powder adsorbent into a copper, lead and cadmium heavy metal ion solution with a certain concentration, magnetically stirring, sampling at intervals, filtering, preparing a solution with a certain concentration, measuring the content of heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate powder for adsorbing the heavy metal ions.
Wherein the dosage of the nano calcium titanate is 1 g.
Wherein the heavy metal pollutants mainly refer to copper ions, lead ions and cadmium ions; the adsorption temperature is 20-50 ℃, and the adsorption time is 5 h.
Wherein the concentration ranges of the copper ions, the copper ions and the cadmium ions are all 400mg/L at 200-.
The nano calcium titanate adsorbent has the effect of adsorbing heavy metal ions, the effect of adsorbing the heavy metal ions is better along with the rise of the temperature, and the nano calcium titanate used as the adsorbent can respectively adsorb copper ions, lead ions and cadmium ions to reach 69.7mg/g, 175.9mg/g and 65.9 mg/g.
The invention has the advantages that: the invention firstly takes metatitanic acid and calcium hydroxide as raw materials, and prepares the nano calcium titanate by a hydrothermal synthesis method, the higher the hydrothermal synthesis temperature is, the better the morphology of the formed nano calcium titanate is, the particle size is 800nm, the invention discovers that the temperature has important influence on the crystal structure of the nano calcium titanate, and the high temperature is beneficial to the formation of perfect calcium titanate crystals. Meanwhile, when the prepared nano calcium titanate with a perfect crystal structure is used as an adsorbent to treat wastewater containing heavy metal ions, the excellent adsorption effect is shown. The nano calcium titanate provided by the patent has the advantages of simple preparation process, safe reaction and low raw material price; the nano calcium titanate is used for adsorbing heavy metal ions in sewage, the adsorption effect is good, the heavy metal ions in the sewage, especially lead ion pollution, can be effectively adsorbed, and the method has good economic and environmental benefits and wide application prospect in the aspect of sewage treatment.
Drawings
FIG. 1 is an electron microscope scanning image of a sample of nano calcium titanate powder prepared in example 1.
FIG. 2 is an electron microscope scanning image of the nano calcium titanate powder sample prepared in example 4.
FIG. 3 is an electron microscope scanning image of the nano calcium titanate powder sample prepared in example 6.
Detailed Description
The invention is further described below with reference to specific embodiments and the accompanying drawings.
Example 1:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50mL of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 12 hours at 120 ℃. Taking out the reaction product, vacuum filtering with distilled water to neutrality, and drying in 80 deg.C oven to obtain nanometer calcium titanate powder (named CaTiO)3-1). Particle size 300nm, as shown in FIG. 1.
1g of CaTiO is taken3-1, adding the calcium titanate into 250mL of heavy metal ion solution of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L) with certain concentration, magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 1 CaTiO3-1 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 2:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50mL of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 12 hours at 140 ℃. Taking out the reaction product, vacuum filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain nanometer calcium titanate powder, and recording as CaTiO3-2. Particle size340nm。
1g of CaTiO is taken3-2, adding the calcium titanate into 250mL of heavy metal ion solution of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L) with certain concentration, magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 2 CaTiO3-2 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 3:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 12 hours at 160 ℃. Taking out the reaction product, vacuum filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain nanometer calcium titanate powder, and recording as CaTiO3-3. The grain diameter is 375 nm.
1g of CaTiO is taken3-3, adding the calcium titanate into 250mL of heavy metal ion solution with certain concentration of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L), magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 3 CaTiO3-3 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 4:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 12 hours at 180 ℃. Taking out the reaction product, vacuum-filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain adsorbent named CaTiO3-4. Particle size 800nm, as shown in FIG. 2.
1g of CaTiO is taken3-4, adding the calcium titanate into 250mL of heavy metal ion solution of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L) with certain concentration, magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 4 CaTiO3-4 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 5:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 10 hours at 160 ℃. Taking out the reaction product, vacuum-filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain adsorbent named CaTiO3-5. The particle size is 355 nm.
1g of CaTiO is taken3-5 adding 250mL of heavy metal ion solution of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L) with a certain concentration, magnetically stirring, sampling at intervals, filteringThen preparing a solution with a certain concentration, measuring the content of heavy metal ions in the solution by using an atomic absorption spectrophotometer, and obtaining the nano CaTiO through calculation3The adsorption amount of adsorbed heavy metal ions is shown in the following table.
TABLE 5 CaTiO3-5 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 6:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 16 hours at 160 ℃. Taking out the reaction product, vacuum-filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain adsorbent named CaTiO3-6. Particle size 395nm, as shown in FIG. 3.
1g of CaTiO is taken3-6, adding the calcium titanate into 250mL of heavy metal ion solution with certain concentration of copper (400mg/L), lead (900mg/L) and cadmium (400mg/L), magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 6 CaTiO3-6 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 7:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) is placed in a 1L plastic beaker, 450mL of distilled water is added, magnetic stirring is carried out for 15min, and 2.5mol/L sodium hydroxide solution is added into the beakerSex (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 14 hours at 160 ℃. Taking out the reaction product, vacuum-filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain adsorbent named CaTiO3-7. The particle size is 380 nm.
1g of CaTiO is taken3-7, adding the calcium titanate into 250mL of heavy metal ion solution with certain concentration of copper (200mg/L), lead (700mg/L) and cadmium (200mg/L), magnetically stirring, sampling at intervals, filtering to prepare solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 7 CaTiO3-7 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Example 8:
55.6g of metatitanic acid starting material (solid content: TiO)220g, 0.25mol) in a 1L plastic beaker, adding 450mL of distilled water, magnetically stirring for 15min, and dropwise adding 2.5mol/L sodium hydroxide solution to neutral (pH 7); 19.3g (95%, 0.25mol) of calcium hydroxide are dispersed in 50ml of distilled water, added to the metatitanic acid suspension and stirred for a further 2 h. Transferring the mixture into a hydrothermal reaction kettle, and reacting for 14 hours at 160 ℃. Taking out the reaction product, vacuum-filtering with distilled water to neutrality, drying in 80 deg.C oven to obtain adsorbent named CaTiO3-7. The particle size is 380 nm.
1g of CaTiO is taken3-8, adding the calcium titanate into 250mL of heavy metal ion solution with certain concentration of copper (300mg/L), lead (800mg/L) and cadmium (300mg/L), magnetically stirring, sampling at intervals, filtering, preparing solution with certain concentration, measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer, and calculating to obtain the adsorption capacity of the nano calcium titanate for adsorbing the heavy metal ions as shown in the following table.
TABLE 8 CaTiO3-8 adsorption capacity for heavy metal ions (adsorption time ═ 5h)
Claims (4)
1. A preparation method of a nano calcium titanate powder adsorbent is characterized in that the adsorbent is prepared by the following steps:
placing a certain amount of metatitanic acid raw material in a plastic beaker, adding a certain amount of distilled water, uniformly stirring to obtain metatitanic acid slurry, and dropwise adding a sodium hydroxide solution with a certain concentration to neutrality; dispersing a certain amount of calcium hydroxide in distilled water with a certain volume, adding the calcium hydroxide into the metatitanic acid suspension, continuously stirring, and transferring the calcium hydroxide into a hydrothermal reaction kettle; after the hydrothermal reaction is carried out for a period of time, taking out a reaction product, carrying out suction filtration by using distilled water to neutrality, placing the reaction product in an oven for drying, and storing the prepared nano calcium titanate powder;
the amount of the metatitanic acid raw material is 55.6g, and the amount of the distilled water is 450 mL;
the Ca (OH)2In an amount of Ca (OH)2Preparing a slurry according to the molar ratio of Ca to Ti =1 to 1 in metatitanic acid; the mass fraction of metatitanic acid in the metatitanic acid raw material is 36 percent (by TiO)2Meter), the balance being water;
the hydrothermal reaction temperature is 120-160 ℃, and the hydrothermal reaction time is 10-16 h.
2. The method for preparing the nano calcium titanate powder adsorbent according to claim 1, wherein the concentration of the sodium hydroxide is 2.5 mol/L.
3. The nano calcium titanate powder adsorbent prepared by the preparation method according to any one of claims 1-2, wherein the nano calcium titanate powder adsorbent has a calcium titanate crystal structure and has a particle size of 300-800 nm.
4. The application of the nano calcium titanate powder adsorbent in adsorbing copper ions, lead ions or cadmium ions in wastewater according to claim 3, wherein the adsorption temperature of the nano calcium titanate powder adsorbent in adsorbing heavy metal ions in wastewater is 20-50 ℃; the concentration ranges of the copper ions and the cadmium ions are both 200-400mg/L, and the concentration range of the lead ions is 700-900 mg/L.
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