CN113522224B - Method for preparing calcium titanate adsorption material by using low-grade rutile concentrate - Google Patents
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Abstract
The invention discloses a method for preparing a calcium titanate adsorbing material by using low-grade rutile concentrate. The method is used for preparing the calcium titanate adsorbing material with stable crystal structure and excellent stability. The low-grade rutile has wide sources and low price, can comprehensively utilize the titanium dioxide resource, changes waste into valuable, and solves the problem of ecological environment pollution. Meanwhile, calcium chloride and potassium silicate are used as molten salt reaction media, so that the temperature of a reaction system can be effectively reduced, and the cost is saved. The produced high value-added product can effectively remove heavy metal ions in the sewage, has wide application prospect in the field of sewage treatment, and has good economic benefit, environmental benefit and social benefit.
Description
Technical Field
The invention belongs to the technical field of powder material preparation, and particularly relates to a method for preparing a calcium titanate adsorption material by using low-grade rutile concentrate.
Background
Rutile is one of the main minerals for refining metallic titanium and manufacturing titanium dioxide, rutile ore in China has the characteristics of low grade, fine granularity, complex mineral composition and distribution relation, poor selectivity and the like, so that the grade of rutile concentrate is low, the utilization difficulty is increased, a large amount of low-grade rutile concentrate products are stacked, a large amount of land is occupied, and the ecological environment is polluted. Therefore, the practical significance of the realization of the maximization of the comprehensive utilization of resources is important on how to fully utilize the rutile concentrate resources to prepare high-added-value products. The patent "a method for preparing aluminum titanate refractory material with industrial aluminum slag and titanium slag (CN 202010776149)" mixes industrial aluminum slag and titanium slag uniformly and then calcines them to prepare the aluminum titanate refractory material, thus changing the resources into valuable and solving the problem of ecological environment pollution. The patent ' a comprehensive utilization method of titanium slag ' (CN 201910140636) ' prepares nano titanium dioxide from molten slag of a titanium-containing electric furnace through alkali fusion, water leaching and calcination, and achieves the purposes of effectively utilizing titanium slag resources and relieving the environmental pollution and harm of the titanium slag.
The low-grade rutile concentrate is produced by the low grade, fine granularity, complex mineral composition and distribution relation of original rutile ore and the limitation of separation technology, and the low-grade rutile concentrate is accumulated because high-end titanium materials cannot be prepared by further utilizing the low-grade rutile concentrate, thereby occupying a large amount of land resources. This not only affects the ecological environment, but also causes waste of resources, and at the same time makes the use of titanium dioxide, which is the main chemical component, unreasonable. With the increase of the urbanization process and the rapid development of the industrial technology, a great amount of solid wastes including low-grade rutile concentrates are accumulated, so that a series of ecological environment problems such as heavy metal pollution are brought. The problem of heavy metal pollution can be solved by adopting a porous adsorbent and an adsorption method so as to achieve the aim of purifying water quality. 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.
Disclosure of Invention
The invention aims to provide a method for preparing a calcium titanate adsorbing material by using low-grade rutile concentrate.
A method for preparing a calcium titanate adsorption material by using low-grade rutile concentrate comprises the following steps:
(1) mixing 40-50% of low-grade rutile concentrate, 30-40% of calcium oxide and 10-20% of molten salt agent in percentage by mass, and grinding the mixture in a ball milling tank for 0.5-2h to obtain a mixed material;
(2) pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm by a tablet press under 10-30 Mpa;
(3) placing the material pieces into a muffle furnace at the temperature of 700-900 ℃ for roasting for 1-3h, and naturally cooling along with the furnace;
(4) washing the roasted material with deionized water until no Cl is formed-And drying to obtain the calcium titanate powder material.
The molten salt agent is calcium chloride and potassium silicate according to the weight ratio of 1: 1, mixing the mixture.
The granularity of the low-grade rutile concentrate is 10-70 mu m.
The low-grade rutile concentrate comprises the following chemical components in percentage by mass: TiO 22The content is 75-85%.
The heavy metal ions are one or more of copper ions, lead ions and cadmium ions.
The adsorption temperature of the calcium titanate adsorption material for adsorbing heavy metal ions in the wastewater is 25-45 ℃; the concentration ranges of the copper ions and the cadmium ions are both 300-400mg/L, and the concentration range of the lead ions is 600-800 mg/L.
The invention has the beneficial effects that: the invention adopts low-grade rutile concentrate as the raw material, reduces the loss of titanium dioxide resources, regenerates the titanium dioxide resources into calcium titanate powder materials with good adsorption performance, realizes the maximization of the comprehensive utilization of the titanium resources, effectively removes heavy metal ions in sewage, solves the problem of ecological environment, achieves the purposes of treating wastes with processes of wastes against one another and establishes a win-win mode system integrating economic benefits and environmental protection benefits. Secondly, the calcium titanate powder material prepared by the technology has the advantages of wide raw material source, low price, simple technical route and strong production process operability, and the mixture of calcium chloride and potassium silicate is added in the preparation process and is used as a molten salt reaction medium to accelerate the contact and flow of materials in the reaction process, improve the reaction activity, greatly reduce the temperature of a reaction system, reduce the reaction energy consumption and further reduce the production cost. Finally, the calcium titanate powder material prepared by the invention has excellent adsorption performance, can effectively remove heavy metal ions in sewage, and has wide application prospect in the aspect of sewage treatment.
Drawings
FIG. 1 is a process flow diagram for preparing calcium titanate powder according to the present invention.
FIG. 2 is an XRD pattern of a sample of calcium titanate powder prepared in example 1 of the present invention.
FIG. 3 is an XRD pattern of a sample of calcium titanate powder prepared in example 2 of the present invention.
FIG. 4 is an electron microscope scan of a sample of calcium titanate powder prepared in example 3 of the present invention.
FIG. 5 is an electron microscope scan of a sample of calcium titanate powder prepared in example 1 of the present invention.
Detailed Description
In order that the invention may be more fully understood, reference will now be made to the following description. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein. Rather, these embodiments are provided so that this disclosure will be thorough and complete.
The following examples use low grade rutile concentrate as the raw material, and the chemical composition of the raw material is shown in table 1 below:
TABLE 1 chemical composition of the raw materials
The process flow for preparing calcium titanate powder is shown in figure 1.
Example 1
4g of low-grade rutile concentrate with the granularity of 70 mu m, 2.8g of analytically pure calcium oxide, 1g of analytically pure calcium chloride and 1g of analytically pure potassium silicate are mixed and put into a ball milling tank for grinding for 1 hour; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material pieces into a muffle furnace at 750 ℃ for roasting for 2h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-And drying to obtain the calcium titanate powder material.
Adding 1g of calcium titanate powder material into 250mL of heavy metal ion solution containing copper (300mg/L), lead (600mg/L) and cadmium (300mg/L), carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the calcium titanate for adsorbing the heavy metal ions.
The XRD pattern and the electron scanning pattern of the calcium titanate powder prepared in the example are shown in FIG. 2 and FIG. 5 respectively; the adsorption capacity (adsorption time: 4h) for heavy metal ions is shown in Table 2.
TABLE 2 adsorption capacity of calcium titanate for heavy metal ions (adsorption time 4h)
Example 2
4g of low-grade rutile concentrate with the granularity of 70 mu m, 2.8g of analytically pure calcium oxide, 1g of analytically pure calcium chloride and 1g of analytically pure potassium silicate are mixed and put into a ball milling tank for grinding for 1 hour; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material slices into a muffle furnace at 800 ℃ for roasting for 3h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-And drying to obtain the calcium titanate powder material.
Adding 1g of calcium titanate powder material into 250mL of solution containing copper (400mg/L), lead (800mg/L) and cadmium (400mg/L) heavy metal ions, carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the calcium titanate for adsorbing the heavy metal ions.
The XRD pattern of the calcium titanate powder prepared in this example is shown in FIG. 3, and the adsorption capacity (4 h adsorption time) of the powder to heavy metal ions is shown in Table 3.
TABLE 3 adsorption capacity of calcium titanate for heavy metal ions (adsorption time 4h)
Example 3
Mixing 5g of low-grade rutile concentrate with the granularity of 70 mu m, 3g of analytically pure calcium oxide and 2.4g of analytically pure calcium chloride, and putting the mixture into a ball milling tank for grinding for 2 hours; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; and (3) putting the material sheet into a muffle furnace at 900 ℃ for roasting for 3h, naturally cooling along with the furnace, repeatedly washing the roasted material with deionized water until no Cl & lt- & gt exists, and drying to obtain the calcium titanate powder material.
Adding 1g of calcium titanate powder material into 250mL of solution containing copper (350mg/L), lead (700mg/L) and cadmium (350mg/L) heavy metal ions, carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the calcium titanate for adsorbing the heavy metal ions.
An electron microscope scanning image of the calcium titanate powder prepared in this example is shown in FIG. 4, and the adsorption capacity (adsorption time: 4h) for heavy metal ions is shown in Table 4.
TABLE 4 adsorption capacity of calcium titanate for heavy metal ions (adsorption time 4h)
Comparative example 1
Mixing 4g of low-grade rutile concentrate with the granularity of 70 mu m, 2.8g of analytically pure calcium oxide and 2g of analytically pure calcium chloride, and grinding the mixture in a ball-milling tank for 1 hour; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material pieces into a muffle furnace at 750 ℃ for roasting for 2h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-And drying to obtain the calcium titanate powder material, wherein the calcium titanate powder material is reddened by visual inspection, incomplete in reaction and poor in quality.
Adding 1g of calcium titanate powder material into 250mL of heavy metal ion solution containing copper (300mg/L), lead (600mg/L) and cadmium (300mg/L), carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the calcium titanate for adsorbing the heavy metal ions.
The adsorption capacity (adsorption time: 4h) of the calcium titanate powder prepared in this example for heavy metal ions is shown in Table 5.
TABLE 5 adsorption capacity of calcium titanate for heavy metal ions (adsorption time 4h)
Comparative example 2
Mixing 4g of low-grade rutile concentrate with the granularity of 70 mu m, 2.8g of analytically pure calcium oxide and 2g of analytically pure potassium silicate, and grinding the mixture in a ball-milling tank for 1 hour; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material pieces into a muffle furnace at 750 ℃ for roasting for 2h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-And drying to obtain the calcium titanate powder material, wherein the calcium titanate powder material is reddened by visual inspection, incomplete in reaction and poor in quality.
Adding 1g of calcium titanate powder material into 250mL of heavy metal ion solution containing copper (300mg/L), lead (600mg/L) and cadmium (300mg/L), carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the calcium titanate for adsorbing the heavy metal ions.
The adsorption capacity (adsorption time: 4h) of the calcium titanate powder prepared in this example for heavy metal ions is shown in Table 6.
TABLE 6 adsorption capacity of calcium titanate for heavy metal ions (adsorption time 4h)
Comparative example 3
4g of low grade rutile concentrate having a particle size of 70 μm, 2.8g of analytically pure calcium oxide, 1g of analytically pure calcium oxideMixing pure calcium chloride and 1g of analytically pure potassium silicate, and grinding for 1 hour in a ball milling tank; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material pieces into a muffle furnace at 700 ℃ for roasting for 2h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-Drying, visual inspection does not obtain calcium titanate powder, reaction is incomplete, and the measured adsorption capacity of the final product to heavy metal ions is almost zero.
Example 4
Mixing 4g of low-grade rutile concentrate with the granularity of 70 mu m, 2.8g of analytically pure calcium oxide, 1g of abalone shell, 1g of analytically pure calcium chloride and 1g of analytically pure potassium silicate, and putting the mixture into a ball milling tank for grinding for 1 hour; pressing the mixed material into material tablets with the diameter of 20mm and the height of 10mm under the pressure of 30Mpa by a tablet press; placing the material slices into a muffle furnace at 800 ℃ for roasting for 3h, naturally cooling along with the furnace, and repeatedly washing the roasted material with deionized water until no Cl exists-And (4) drying to obtain the adsorption powder material.
Adding 1g of the adsorption powder material into 250mL of a solution containing copper (400mg/L), lead (800mg/L) and cadmium (400mg/L) heavy metal ions, carrying out magnetic stirring, sampling at intervals, filtering, taking the solution, and measuring the content of the heavy metal ions in the solution by using an atomic absorption spectrophotometer to obtain the adsorption capacity of the adsorption powder for adsorbing the heavy metal ions.
The adsorption capacity (adsorption time: 4h) of the adsorption powder for heavy metal ions prepared in this example is shown in Table 7.
TABLE 7 adsorption capacity of the adsorption powder for heavy metal ions (adsorption time 4h)
The adsorption powder not only generates calcium titanate powder, but also finally generates a part of calcium titanate and carbon hydroxyapatite mixed crystal powder structure and other unknown structures through the complex components of the abalone shell, thereby promoting the absorption of heavy metal ions. The inventor also adopts other analogues such as egg shells, spiral shells, clam shells and the like to replace abalone shells to carry out the preparation of the adsorption powder and adsorption experiments, and the adsorption capacity of the adsorption powder to heavy metal ions cannot be improved.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent should be subject to the appended claims.
Claims (5)
1. A method for preparing a calcium titanate adsorption material by using low-grade rutile concentrate is characterized by comprising the following steps:
(1) mixing 40-50% of low-grade rutile concentrate, 30-40% of calcium oxide and 10-20% of molten salt agent in percentage by mass, and grinding the mixture in a ball milling tank for 0.5-2h to obtain a mixed material;
(2) pressing the mixed material into a material sheet with the diameter of 20mm and the height of 10mm by a tablet press under the pressure of 10-30 MPa;
(3) placing the material pieces into a muffle furnace at the temperature of 700-900 ℃ for roasting for 1-3h, and naturally cooling along with the furnace;
(4) washing the roasted material with deionized water until no Cl is formed-Drying to obtain calcium titanate powder material;
the molten salt agent is calcium chloride and potassium silicate according to the mass ratio of 1: 1, mixing the mixture.
2. The method of using low-grade rutile concentrate to produce a calcium titanate adsorbent material of claim 1, wherein the low-grade rutile concentrate has a particle size of 10-70 μm.
3. The method of using low-grade rutile concentrate to produce a calcium titanate adsorbent material of claim 1, wherein the low-grade rutile concentrate has a chemical compositionIn the formula (I), the mass percentages are as follows: TiO 22The content is 75-85%.
4. The application of the calcium titanate adsorbing material prepared by the method according to claim 1 in adsorbing heavy metal ions in wastewater, wherein the heavy metal ions are one or more of copper ions, lead ions and cadmium ions.
5. The use according to claim 4, wherein the adsorption temperature of the calcium titanate adsorption material for adsorbing heavy metal ions in wastewater is 25-45 ℃; the concentration ranges of the copper ions and the cadmium ions are both 300-400mg/L, and the concentration range of the lead ions is 600-800 mg/L.
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| CN101787431B (en) * | 2010-02-02 | 2011-09-14 | 昆明理工大学 | Method for preparing acid-soluble titanium slag by high titanium slag through microwave irradiation |
| CN101787432B (en) * | 2010-02-02 | 2011-09-14 | 昆明理工大学 | Method for preparing acid-soluble titanium slag from high-titanium slag |
| CN102430382A (en) * | 2011-09-23 | 2012-05-02 | 沈阳理工大学 | Method for preparing porous calcium titanate heavy metal adsorbent |
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