CN112661193B - Method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings - Google Patents
Method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings Download PDFInfo
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Abstract
The invention discloses a method for preparing binary and ternary high-performance composite aerogel by using iron tailings, which comprises the following steps: mixing iron tailings and sodium hydroxide, carrying out alkali fusion activation, cooling, washing with deionized water for solid-liquid separation, standing and layering washing liquor, separating supernatant from lower-layer mixed liquor, adding an acid catalyst under an alkaline condition, standing and aging to obtain wet gel, carrying out solvent replacement on the wet gel, and drying under normal pressure to obtain the binary and ternary composite aerogel. The invention takes the iron tailings as raw materials, has low price, wide sources, mild preparation conditions, simple process and low equipment requirement, is easy to realize industrialized preparation, and can simultaneously obtain binary and magnetic ternary composite silicon-based aerogel; the tap density of the prepared aerogel is less than 0.20g/cm3Wherein the specific surface areas of the binary aerogel and the ternary aerogel can reach 986m respectively2G and 612m2The adsorption capacity to methylene blue is more than 300 mg/g.
Description
Technical Field
The invention relates to a method for simultaneously preparing binary and ternary composite aerogel by taking iron tailings as raw materials, belonging to the field of aerogel preparation.
Background
SiO2The aerogel is a nano material with a three-dimensional reticular porous structure and formed by combining nano silicon dioxide particles, has higher specific surface area, extremely low density and lower normal temperature heat conductivity, and has the functions of heat preservation, heat insulation, adsorption and CO absorption2The catalyst has good application prospect in many fields such as isolation, catalyst carrier, aerospace and the like. The main preparation process of silica aerogels usually involves two typical steps, sol-gel and drying, separatelyIn order to form and maintain the gel three-dimensional structure to the maximum extent, so that an aerogel product is finally obtained, currently, a recognized mature process usually uses Tetraethoxysilane (TEOS) as a silicon source and obtains silica aerogel through supercritical drying, but the existing process still has many challenges in the aspects of technology and application, for example, the TEOS silicon source is high in price, the supercritical drying equipment is strict in requirement, the technical difficulty is high, and the large-scale industrial popularization is not facilitated, so that the practical significance of finding a cheaper silicon source and a simpler and more convenient drying mode is great in order to overcome the defects.
The iron tailings are wastes after mineral separation and are the main components of industrial solid wastes. At present, the comprehensive utilization rate of tailings in China is only 7%, and the quantity of iron tailings stored in a stockpile mode is up to billions of tons, which accounts for about 1/3 of the total quantity of all tailings stored in a stockpile mode. Therefore, the comprehensive recycling problem of the iron tailings has received extensive attention of the whole society. Generally, the iron tailings mainly contain silica, alumina, iron oxide, magnesium oxide and calcium oxide with the largest content, and the balance of a small amount of associated element oxides, and at present, the utilization of the iron tailings is mainly in the aspects of tailing recleaning, goaf filling in mining areas, tailing building materials, soil conditioners and the like, and although the methods can solve the problem of partial tailing stockpiling in quantity, the methods still need to be researched and popularized in the aspect of related high-value-added products with more market competitiveness, which is not favorable for efficient resource utilization of the iron tailings. The silicon dioxide in the iron tailings is a natural silicon source, and can be extracted to serve as a raw material for preparing the high-added-value silicon dioxide aerogel after alkali treatment, so that the comprehensive utilization efficiency of the iron tailings can be improved while the green ecological development is realized. Meanwhile, alumina and iron oxide in tailings are also potential raw materials for preparing the aerogel, generally, the content of the valuable elements is relatively low, the process is complex and the cost is high when the valuable elements are independently purified or utilized, so that the valuable elements are reserved in the aerogel as essential components and are compounded with silicon dioxide to prepare the composite aerogel, and the synergistic and functionalized effect is achieved. Currently, there are few reports related to the preparation of aerogel by using silica in tailings, and publication No. CN108658130A discloses a method for simultaneously preparing iron oxide and silica aerogel from iron tailings, which includes acid elution of iron and alkali fusion extraction of silicon to obtain an iron source and a silicon source, respectively, but does not solve the problem of preparing a composite material by combining the two; publication No. CN109133072A discloses a method for preparing hydrophobic silica aerogel by using iron tailings as raw materials at ultra-fast speed, and publication No. CN109012517A discloses a method for preparing composite silicon-based aerogel by using iron tailings as raw materials, although the composite material of alumina and silica is obtained to a certain extent by the alkali fusion process, the iron oxide is still remained in the alkali fusion slag due to the low initial alkali fusion treatment temperature, and the iron oxide in the tailings cannot be extracted to prepare the iron oxide/silica aerogel composite material.
Disclosure of Invention
Aiming at the technical problems in the prior art, the invention aims to provide a method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings, which takes solid waste iron tailings as a raw material, has the advantages of low price, wide sources, mild preparation conditions, simple process, low equipment requirement and easy realization of industrialized preparation, and can simultaneously obtain binary composite aerogel and ternary magnetic composite aerogel. The tap density of the prepared aerogel is less than 0.20g/cm3The average pore diameter is 5.25-8.67nm, wherein the specific surface area of the binary composite aerogel can reach 986m2The/g can be used as an excellent carrier catalyst, and the specific surface area of the ternary magnetic composite aerogel can reach 600m2The adsorption capacity of the adsorbent to methylene blue exceeds 300mg/g, the adsorption performance is excellent, the separation is easy, and both the adsorption capacity and the separation have good application potential.
In order to solve the technical problems, the technical scheme adopted by the invention is as follows:
the method for simultaneously preparing the binary and ternary high-performance composite aerogel by using the iron tailings comprises the following steps: (1) uniformly mixing iron tailings serving as a raw material with powder sodium hydroxide, placing the mixture in a muffle furnace, heating, preserving heat, reacting completely, cooling to room temperature, washing the obtained mixture with deionized water for 4-10 times, and collecting washing liquor; (2) placing the washing liquor obtained in the step (1) in a container, standing for 10-60 minutes until the washing liquor is obviously layered, sucking out supernatant liquor by using a suction pipe, respectively adding an acidic catalyst into the supernatant liquor and the lower mixed liquor, respectively adjusting the pH of the washing liquor to 9-10.5, standing until massive gel is formed, respectively taking out the gel, placing the gel in deionized water, continuously aging for 12-24 hours to obtain wet gel, and replacing the deionized water for 3-6 times in the aging process; (3) respectively placing the wet gel obtained in the step (2) in a displacer solution for 12-24 hours to perform solvent displacement, and replacing fresh displacer solution every 2-6 hours to completely remove water and other residual reagents in the wet gel; (4) and (4) respectively taking out the wet gel after the solvent replacement in the step (3), and drying at normal pressure to obtain the binary composite aerogel and the ternary magnetic composite aerogel.
The iron tailings are powder, have the granularity of more than 50 meshes, and contain silicon dioxide, aluminum oxide, iron oxide, magnesium oxide, calcium oxide, potassium oxide and sodium oxide.
In the step (1), the mass ratio of the iron tailings to the sodium hydroxide is 1:1-3, the water consumption for flushing the cooled mixture each time is 1:20-100 (g/ml) of the mass ratio of the mixture to the volume of water, and the operation temperature is room temperature.
The heating temperature in the step (1) is 700-.
In the step (2), the used acidic catalyst is a gel catalyzed by phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid or citric acid solution selected from the supernatant, the mass fraction of the used acid solution is 2-15%, the mixed solution of the lower layer is a gel catalyzed by phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid or citric acid solution matched with pure tartaric acid or pure ascorbic acid, the mass fraction of the used acid solution is 2-15%, and the mass ratio of tartaric acid, ascorbic acid and other acids is 1: 1-1: 5.
in the step (3), the used displacing agent is one or more of ethanol, tertiary butanol, acetone, methanol and glycol, and the dosage of each time is that the wet gel is at least completely immersed.
The normal pressure drying method in the step (3) is to put the wet gel into an open container, seal the container by using a preservative film, open 5-30 holes with the size of 1x1mm on the preservative film so as to regulate and control the drying rate of the wet gel in the drying process and reduce the collapse of a gel framework, and finally place the container in an oven to be dried for 24-72 hours at the temperature of 50-150 ℃ until the wet gel is completely dried.
The tap density of the binary composite aerogel and the ternary magnetic composite aerogel obtained in the step (4) is 0.158-0.194g/cm3Specific surface area of 320-986m2The specific molecular weight of the dye is determined by the following formula, wherein the specific molecular weight is determined by the specific molecular weight of the dye, the specific molecular weight is 5.25-8.67nm, and the adsorption capacities of the two to methylene blue of typical dyes can reach 322mg/g and 354mg/g respectively.
The invention has the beneficial effects that:
1. the invention only takes the iron tailings as the raw material, has the advantages of wide source, low price, environmental protection and no toxicity, meets the development requirements of national energy conservation and emission reduction, simultaneously realizes the preparation of the composite material by utilizing the iron oxide and the aluminum oxide in the iron tailings, obtains the silicon-aluminum and silicon-aluminum-iron composite aerogel with high specific surface area and high adsorption performance, and effectively improves the functionality and the added value of the product.
2. According to the invention, through high-temperature alkali fusion treatment, iron oxide in iron tailings is effectively converted into ferrite, the conversion from insoluble iron to soluble iron is realized, and then through a simple sol-gel process, standing layering, solvent replacement and normal-pressure drying treatment, the aluminum-silicon binary composite aerogel and the aluminum-silicon-iron ternary magnetic composite aerogel are obtained in one step, and meanwhile, the silicon dioxide aerogel is synergistically enhanced by utilizing aluminum oxide and iron oxide, so that the silicon-aluminum binary composite aerogel has a developed pore structure and a specific surface area of 986m2The methylene blue adsorption capacity exceeds 300mg/g, and the silicon-aluminum-iron ternary magnetic composite aerogel has a slightly lower specific surface area, but the specific surface area can also exceed 600m2The catalytic oxidation effect of the iron oxide enables the adsorption capacity of the iron oxide to methylene blue to be close to or even higher than that of silicon-aluminum binary composite aerogel, the adsorption capacity exceeds 350mg/g, excellent adsorption potential is embodied, meanwhile, through the sol-gel process and the reduction effect of organic acid, the iron oxide in the ternary magnetic composite aerogel has magnetism, the iron oxide mainly exists in a magnetic gamma iron oxide form, additional magnetic substances are not needed, the magnetic functionalization of an iron source in tailings is realized in one step, and the ternary magnetic composite aerogel material is easier to separate.
3. The process used in the invention does not need an additional silicon source, ion exchange, surface modification, supercritical drying and magnetic additives, realizes aerogel self-composite reinforcement by only using the effective components in the iron tailings, has simple and mild preparation conditions, low equipment requirement, low energy consumption, energy conservation and environmental protection, provides a new idea for utilizing solid waste resources, and is easy for industrial production.
Drawings
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph showing the effect of layering of the washing liquid at rest in example 3;
FIG. 3 is a physical map of the ternary magnetic composite aerogel (left) and binary composite aerogel of example 3;
FIG. 4 is a magnetic display diagram of a ternary magnetic composite aerogel according to example 3;
FIG. 5 is an SEM-EDS image of a composite aerogel of example 3;
FIG. 6 is the composite aerogel XRD pattern of example 3;
figure 7 is the composite aerogel nitrogen adsorption isotherm of example 3.
Detailed Description
The technical solution of the present invention is further explained by the following embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
A method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings comprises the following specific preparation steps: (1) putting the powdery iron tailings with the particle size of more than 50 meshes and powdery sodium hydroxide into a crucible according to the mass ratio of 1:1, uniformly mixing, putting the crucible into a muffle furnace, setting the temperature rise rate of the muffle furnace to be 5 ℃/min, heating to 700 ℃, keeping the temperature for 4 hours to obtain a mixture after the iron tailings and the sodium hydroxide react, and washing the mixture after the reaction and deionized water for 4 times according to the solid mass to liquid volume ratio of 1:20 to obtain washing liquid.
(2) The wash solution was allowed to stand for 30 minutes, whereupon it was clearly separated, and the supernatant was aspirated into another glass container. Adding 5% by mass of hydrochloric acid + ascorbic acid (in a mass ratio of 2: 1) into two containers respectively to adjust the pH of the liquid in the containers to 9.1, and standing the liquid in the two containers until a block gel is formed.
(3) The two block gels were taken out and immersed in deionized water, respectively, and left to stand at room temperature for 16 hours for aging to obtain wet gels, during which deionized water was changed 3 times.
(4) The aged wet gel was taken out and immersed in 90mL of ethanol solvent and left to stand for 20 hours, during which the solvent was replaced 3 times, to completely remove water and residual reagents in the pores of the wet gel.
(5) And taking the wet gel out of the displacement solvent, placing the wet gel in a 500ml beaker, sealing the container opening by using a preservative film, pricking 4 small holes on the preservative film, keeping the wet gel obtained from the supernatant at 85 ℃ for 36 hours under a normal pressure state, and keeping the wet gel obtained from the lower-layer mixed solution at 110 ℃ for 36 hours for drying, thus obtaining the binary composite aerogel and the ternary magnetic composite aerogel.
Example 2
A method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings comprises the following specific preparation steps: (1) putting powdery iron tailings with the particle size of more than 50 meshes and powdery sodium hydroxide into a crucible according to the mass ratio of 1:2, uniformly mixing, putting the crucible into a muffle furnace, setting the temperature rise rate of the muffle furnace to be 5 ℃/min, heating to 780 ℃, keeping the temperature for 3.5 hours to obtain a mixture after the iron tailings and the sodium hydroxide react, and washing the mixture after the reaction and deionized water for 6 times according to the solid mass to liquid volume ratio of 1:30 to obtain washing liquid.
(2) The wash solutions clearly separated after standing for 40 minutes and the supernatant was pipetted into another glass container. Adding 5% by mass of sulfuric acid + ascorbic acid (in a mass ratio of 2: 1) into two containers respectively to adjust the pH of the liquid in the containers to 9.3, and standing the liquid in the two containers until a block gel is formed.
(3) The two block gels were taken out and immersed in deionized water, respectively, and left to stand at room temperature for 20 hours for aging to obtain wet gels, during which deionized water was replaced 4 times.
(4) The aged wet gel was taken out and immersed in 100mL of methanol solvent and left to stand for 22 hours, during which the solvent was changed 5 times to completely remove water and residual reagent in the pores of the wet gel.
(5) And taking the wet gel out of the displacement solvent, placing the wet gel in a 500ml beaker, sealing the opening of the beaker by using a preservative film, pricking 8 small holes on the preservative film, keeping the wet gel obtained from the supernatant at 80 ℃ for 48 hours under a normal pressure state, and keeping the wet gel obtained from the lower-layer mixed solution at 120 ℃ for 48 hours for drying, thus obtaining the binary composite aerogel and the ternary magnetic composite aerogel.
Example 3
A method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings comprises the following specific preparation steps: (1) putting powdery iron tailings with the particle size of more than 50 meshes and powdery sodium hydroxide into a crucible according to the mass ratio of 1:2.5, uniformly mixing, putting the crucible into a muffle furnace, setting the temperature rise rate of the muffle furnace to be 5 ℃/min, heating to 850 ℃, keeping the temperature for 3 hours to obtain a mixture after the iron tailings and the sodium hydroxide react, and washing the mixture after the reaction and deionized water for 8 times according to the solid mass to liquid volume ratio of 1:40 to obtain washing liquid.
(2) The washing solution is obviously layered after standing for 50 minutes, supernatant liquid is sucked into other glass containers, 10 mass percent of phosphoric acid and tartaric acid (in a mass ratio of 3: 1) are respectively added into the two containers to adjust the pH value of the liquid in the containers to be 9.7, and the liquids in the two containers are kept standing until the liquids are distributed to form block gel.
(3) The two block gels were taken out and immersed in deionized water, respectively, and left to stand at room temperature for 18 hours for aging to give wet gels, during which the deionized water was replaced 5 times.
(4) The aged wet gel was taken out and immersed in 120mL of ethylene glycol solvent and left to stand for 24 hours, during which the solvent was changed 7 times to completely remove water and residual reagent in the pores of the wet gel.
(5) And taking the wet gel out of the displacement solvent, placing the wet gel into a 500ml beaker, sealing the opening of the beaker by using a preservative film, binding 12 small holes on the preservative film, keeping the wet gel obtained from the supernatant at 75 ℃ for 60 hours to dry under the normal pressure state, and keeping the wet gel obtained from the lower-layer mixed solution at 120 ℃ for 60 hours to dry, thus obtaining the binary composite aerogel and the ternary magnetic composite aerogel.
Example 4
A method for simultaneously preparing binary and ternary high-performance composite aerogel by using iron tailings comprises the following specific preparation steps: (1) putting powdery iron tailings with the particle size of more than 50 meshes and powdery sodium hydroxide into a crucible according to the mass ratio of 1:3, uniformly mixing, putting the crucible into a muffle furnace, setting the temperature rise rate of the muffle furnace to be 5 ℃/min, heating to 900 ℃, keeping the temperature for 2.5 hours to obtain a mixture after the iron tailings and the sodium hydroxide react, and washing the mixture after the reaction and deionized water for 8 times according to the solid mass to liquid volume ratio of 1:50 to obtain washing liquid.
(2) The wash clearly separated after standing for 58 minutes and the supernatant was pipetted into another glass container. Adding 15% by mass of citric acid + tartaric acid (mass ratio of 3: 1) into two containers respectively to adjust the pH of the liquid in the containers to 10.2, and standing the liquid in the two containers until the liquid is distributed to form block gel.
(3) The two block gels were taken out and immersed in deionized water, respectively, and left to stand at room temperature for 15 hours for aging to obtain wet gels, during which deionized water was replaced 7 times.
(4) The aged wet gel was taken out and immersed in 140mL of t-butanol solvent and left to stand for 21 hours, during which the solvent was replaced 6 times, to completely remove water and residual reagents in the pores of the wet gel.
(5) And taking the wet gel out of the displacement solvent, placing the wet gel into a beaker with the volume of 500ml, sealing the opening of the beaker by using a preservative film, pricking 18 small holes on the preservative film, keeping the wet gel obtained from the supernatant at 70 ℃ for 72 hours under the normal pressure state, and keeping the wet gel obtained from the lower-layer mixed solution at 130 ℃ for 72 hours for drying, thus obtaining the binary composite aerogel and the ternary magnetic composite aerogel.
TABLE 1
It can be seen from table 1 that, according to the difference of the types of the actual acidic catalysts, the specific surface area of the product has more difference, because the concentration and the type of the acid have certain influence on the formation of the binary composite aerogel and the ternary magnetic composite aerogel, and further influence the strength of the colloid three-dimensional network skeleton structure, the skeleton structure of the colloid is more complete under the catalytic action of the medium-strong acid, and the good pore structure is maintained by matching with the displacing agent with small surface tension in the drying process, so that the larger skeleton collapse is not caused. For the ternary magnetic composite aerogel, the specific surface area of a final aerogel product is reduced due to the influence of iron oxide doping in the formation process of a colloid, but the excellent catalytic oxidation effect of the iron oxide can obviously improve the adsorption and purification effect of the ternary aerogel on methylene blue dye, so that the ternary aerogel still has high methylene blue adsorption capacity under the condition of low specific surface area, and is easy to separate magnetically, and a soluble iron salt precursor is difficult to generate under a low-temperature condition, so that the alkali melting temperature is increased to more than 700 ℃ in the alkali melting stage, and the NaOH ratio is properly increased, which is necessary.
Claims (6)
1. The method for simultaneously preparing the binary and ternary high-performance composite aerogel by using the iron tailings is characterized by comprising the following steps of: (1) uniformly mixing iron tailings serving as a raw material with powder sodium hydroxide, placing the mixture in a muffle furnace, heating, preserving heat, reacting completely, cooling to room temperature, heating at the temperature of 700-900 ℃, preserving heat for 1-5 hours, washing the obtained mixture for 4-10 times with deionized water, and collecting washing liquid; (2) placing the washing liquid obtained in the step (1) in a container, standing for 10-60 minutes until the washing liquid is obviously layered, sucking out the supernatant liquid by using a suction pipe, respectively adding an acidic catalyst into the supernatant liquid and the lower layer mixed liquid, respectively adjusting the pH value to 9-10.5, standing until block-shaped gel is formed, respectively taking out the gel, placing the gel in deionized water, continuously aging for 12-24 hours to obtain wet gel, and replacing the deionized water for 3-6 times in the aging process; (3) respectively placing the wet gel obtained in the step (2) in a displacer solution for 12-24 hours to perform solvent displacement, and replacing fresh displacer solution every 2-6 hours to completely remove water and other residual reagents in the wet gel; (4) and (4) respectively taking out the wet gel after the solvent replacement in the step (3), and drying at normal pressure to obtain the binary composite aerogel and the ternary magnetic composite aerogel.
2. The method for preparing binary and ternary high performance composite aerogels according to claim 1, characterized in that: the iron tailings are powder and contain silicon dioxide, aluminum oxide, iron oxide, magnesium oxide, calcium oxide, potassium oxide and sodium oxide.
3. The method for preparing binary and ternary high performance composite aerogels according to claim 1, characterized in that: in the step (1), the mass ratio of the iron tailings to the sodium hydroxide is 1:1-3, the water consumption for flushing the cooled mixture each time is 1 g: 20-100 ml, and the operation temperature is room temperature.
4. The method for preparing binary and ternary high performance composite aerogels according to claim 1, characterized in that: in the step (2), the used acidic catalyst is a gel catalyzed by phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid or citric acid solution selected from the supernatant, the mass fraction of the used acid solution is 2-15%, the mixed solution of the lower layer is a gel catalyzed by phosphoric acid, nitric acid, hydrochloric acid, sulfuric acid or citric acid solution matched with pure tartaric acid or pure ascorbic acid, the mass fraction of the used acid solution is 2-15%, and the mass ratio of tartaric acid, ascorbic acid and other acids is 1: 1-1: 5.
5. the method for preparing binary and ternary high performance composite aerogels according to claim 1, characterized in that: in the step (3), the used displacer is one or more of ethanol, tertiary butanol, acetone, methanol and glycol, and the dosage of each time is that the wet gel is at least completely immersed.
6. The method for preparing binary and ternary high performance composite aerogels according to claim 1, characterized in that: the normal pressure drying method in the step (3) is to put the wet gel into an open container, seal the container by using a preservative film, open 5-30 holes with the size of 1x1mm on the preservative film so as to regulate and control the drying rate of the wet gel in the drying process and reduce the collapse of a gel framework, and finally place the container in an oven to be dried for 24-72 hours at the temperature of 50-150 ℃ until the wet gel is completely dried.
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| CN108911599A (en) * | 2018-07-18 | 2018-11-30 | 浙江工业大学 | A method of iron oxide and aerosil pad are prepared simultaneously from iron tailings |
| CN109012517A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A method of compound silica-based aerogel is prepared by raw material of iron tailings |
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| US3872217A (en) * | 1971-01-25 | 1975-03-18 | Basf Ag | Process for the manufacture of substantially spherical, silica-containing hydrogels |
| US20140007795A1 (en) * | 2012-07-06 | 2014-01-09 | E I Du Pont De Nemours And Company | Treatment of tailings with deionized silicate solutions |
| CN107694490A (en) * | 2017-11-09 | 2018-02-16 | 姚之予 | A kind of preparation method of ferrosilicon composite aerogel |
| CN108658130A (en) * | 2018-07-18 | 2018-10-16 | 浙江工业大学 | A method of preparing iron oxide and aerosil simultaneously from iron tailings |
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| CN109012517A (en) * | 2018-08-28 | 2018-12-18 | 浙江工业大学 | A method of compound silica-based aerogel is prepared by raw material of iron tailings |
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