CN110668452B - Preparation of SiO from fly ash2-Al2O3Method of compounding aerogel materials - Google Patents
Preparation of SiO from fly ash2-Al2O3Method of compounding aerogel materials Download PDFInfo
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- CN110668452B CN110668452B CN201911032171.1A CN201911032171A CN110668452B CN 110668452 B CN110668452 B CN 110668452B CN 201911032171 A CN201911032171 A CN 201911032171A CN 110668452 B CN110668452 B CN 110668452B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B33/00—Silicon; Compounds thereof
- C01B33/113—Silicon oxides; Hydrates thereof
- C01B33/12—Silica; Hydrates thereof, e.g. lepidoic silicic acid
- C01B33/14—Colloidal silica, e.g. dispersions, gels, sols
- C01B33/157—After-treatment of gels
- C01B33/158—Purification; Drying; Dehydrating
- C01B33/1585—Dehydration into aerogels
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F7/00—Compounds of aluminium
- C01F7/02—Aluminium oxide; Aluminium hydroxide; Aluminates
- C01F7/04—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom
- C01F7/06—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process
- C01F7/0693—Preparation of alkali metal aluminates; Aluminium oxide or hydroxide therefrom by treating aluminous minerals or waste-like raw materials with alkali hydroxide, e.g. leaching of bauxite according to the Bayer process from waste-like raw materials, e.g. fly ash or Bayer calcination dust
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
Preparation of SiO from fly ash2‑Al2O3A method for compounding aerogel belongs to the field of mesoporous materials. The method comprises the following steps of taking fly ash as a raw material, uniformly mixing the fly ash with sodium hydroxide, calcining the mixture in a muffle furnace for a certain time to obtain an alkali fusion mixture, mixing and stirring the alkali fusion mixture and a hydrochloric acid solution, and carrying out solid-liquid separation to obtain a liquid phase containing silicon and aluminum; under the condition of continuously stirring at normal temperature, dropwise adding ammonia water into a liquid phase containing silicon and aluminum to promote the liquid phase to carry out gel reaction to obtain wet gel; after aging, washing with deionized water, solvent replacement and drying under normal pressure to obtain SiO2‑Al2O3And (3) compounding the aerogel. In the whole process flow, the solid waste fly ash is utilized with high added value; the cost is low, the flow is short, and the whole preparation period only needs 3 days; synthesized SiO2‑Al2O3The specific surface area of the composite aerogel is about 900m2(ii)/g; after calcining for 2h at 900 ℃, the amorphous structure is still maintained, and the thermal stability is better.
Description
Technical Field
The invention belongs to the field of mesoporous materials, and particularly relates to a method for synthesizing SiO by using fly ash as a raw material2-Al2O3Methods of compounding aerogel materials.
Background
The aerogel is a porous solid material which is formed by a three-dimensional network structure formed by nano particles and filled with air. The porosity can reach 80-99.8%, the typical pore diameter is 1-100nm, and the specific surface area is usually 200-1200 m2(ii) a density in the range of 0.003 to 0.5g/m3((1) A. Soleimani Dorcheh, M.H. Abbasic, Journal of Materials Processing Tech,2008,199(1-3): 10-26.). Due to the characteristics, the aerogel has great application potential in the aspects of heat insulation materials, separation materials, low dielectric constant materials and the like.
With SiO2Or Al2O3Aerogel phase comparison, Al2O3-SiO2The composite aerogel has better high-temperature performance and thermal stability, and has wider application prospect in the field of high-temperature heat insulation. The scholars ((1) James B.Miller, Edmond I.Ko, Catalysis Today,1998,43(1-2):51-67.(2) Xu, Lin, Jiang, Yongggang, Feng, Junzong, et al, Ceramics International,2015,41(1):437 and 442)) adopts aluminum sec-butoxide and ethyl orthosilicate as precursors of an aluminum source and a silicon source respectively to prepare SiO under the condition of supercritical drying2-Al2O3And (3) compounding the aerogel. Gash ((1) Gash A, Journal of Non-Crystalline Solids,2001,285(1): 22-28.) found that organic epoxides such as propylene oxide can effectively trap protons and can convert the valence of inorganic salts of metals above three to [ M (H)2O)x]n+The form of (A) is stable in aqueous solution, can be subjected to ring-opening reaction with epoxide, and can obtain corresponding gel after a series of hydrolysis and polycondensation. This finding opens the way to the preparation of aerogels with metallic inorganic salts. However, at present, Al2O3-SiO2The preparation process of the composite aerogel is complex, the production cost is high, and the use of a metal alkoxide which is difficult to store and a supercritical drying process with a high risk coefficient is involved, so that the composite aerogel is difficult to be used for industrial production. Based on the method, the low-cost metal inorganic salt or solid waste is used for preparing Al by combining with the normal pressure drying process2O3-SiO2The study of composite aerogels has become a hotspot in recent years in this field ((1) Hu, Wenbin, Li, Mengmeng, Chen, Wei, et al, Colloids and Surfaces A physical and Engineering applications, 2016,501:83-91.(2) Jinmeng Zhu, Shaohui Guo, Xuanhua Li, RSC Advances,2015,5(125): 103656-.
The fly ash is the waste discharged by coal-fired power plants, is one of the largest solid wastes discharged in the world, has the average utilization rate of only 16 percent worldwide, causes the accumulation of a large amount of fly ash, occupies cultivated land and seriously pollutes the environment. The fly ash comprises silicon oxide and aluminum oxide (the sum of the silicon oxide and the aluminum oxide accounts for more than 80%), so that the fly ash is used as a raw material to prepare SiO2-Al2O3Methods of compounding aerogels are promising. However, no studies have been reported.
Based on the analysis, the silicon-aluminum element in the fly ash is extracted by adopting an alkali fusion-acid leaching method, and the SiO is prepared by utilizing a leaching solution in combination with a sol-gel method and a normal pressure drying method2-Al2O3And (3) compounding the aerogel. Book (I)SiO prepared by the invention2-Al2O3The specific surface area of the composite aerogel is as high as 900m2The whole process is simple and easy to implement and only needs 3 days. After calcination at 900 ℃, the aerogel still maintains the amorphous structure, which indicates that the prepared SiO2-Al2O3The composite aerogel can withstand high temperatures of 900 ℃. The invention realizes the high value-added utilization of the fly ash and finds a cheap raw material for the preparation of the aerogel.
The invention content is as follows:
on the basis of completing the leaching of silicon and aluminum by aiming at the fly ash, the invention adopts a sol-gel method to obtain wet gel from the leaching solution containing silicon and aluminum, and adopts a simpler and safer normal pressure drying method to prepare SiO2-Al2O3And (3) compounding the aerogel.
Synthesis of SiO from fly ash2-Al2O3The method for compounding aerogel material is characterized in that under the condition of continuously stirring at room temperature, the SiO is obtained by adding ammonia water into a liquid phase containing silicon and aluminum, aging for a period of time, washing with deionized water, replacing solvent and drying under normal pressure2-Al2O3Composite aerogels, SiO2-Al2O3The composite aerogel synthesis steps are as follows:
(1) the fly ash and a proper amount of sodium hydroxide are uniformly mixed and calcined in a muffle furnace for a certain time to obtain an alkali fusion mixture.
(2) And mixing and stirring the alkali fusion mixture and a hydrochloric acid solution, and performing solid-liquid separation to obtain a liquid phase containing silicon and aluminum.
(3) Under the condition of stirring at room temperature, dropwise adding a proper amount of ammonia water into a liquid phase containing silicon and aluminum to obtain wet gel;
(4) aging the gel obtained in step (3) at room temperature for a period of time;
(5) washing the gel obtained in the step (4) with deionized water;
(6) and (3) carrying out solvent replacement on the washed gel by using absolute ethyl alcohol, and drying the wet gel subjected to solvent replacement in an oven.
Further, the temperature of the muffle furnace in the step (1) is 350-500 ℃, and the temperature is kept for 1-2 h.
Further, the liquid-solid ratio (ml/g) of the deionized water added in the step (2) to the alkali melt mixture is in the range of: 6-8, the liquid-solid ratio (ml/g) of the hydrochloric acid (5mol/L) and the alkali melt mixture is as follows: 5-8.
Further, in the step (3), the pH of the solution is controlled to be 2.7-3.1 by dropwise adding ammonia water (0.25-0.5 mol/L).
Further, the gel in step (4) is aged for 1 to 3 days.
Further, the step (6) requires replacing with anhydrous ethanol solvent for 2-4 times, and drying wet gel in an oven at 40-50 deg.C for 2-4 hr, at 50-65 deg.C for 5-10 hr, and at 65-70 deg.C for 10-14 hr. The purpose of drying gradually at different temperatures is to ensure the integrity of the internal network framework of the aerogel and prevent the internal network framework of the aerogel from collapsing due to too high drying speed.
The whole process flow is energy-saving and low-consumption, is simple and feasible, the whole period only needs 3 days, and the high added value utilization of the fly ash is realized. Prepared SiO2-Al2O3Composite aerogel with specific surface area up to 900m2The temperature of the alloy can be 900 ℃.
The invention has the advantages that: the high added value utilization of the fly ash is realized, the whole preparation process is energy-saving and low in consumption, and the process is short and only needs 3 days. Synthesis of SiO with pure reagents2-Al2O3Compared with the composite aerogel, the invention has low cost and short process. Realizes the preparation of SiO with high specific surface area by the fly ash2-Al2O3The composite aerogel provides a new idea for the high added value utilization of the fly ash while finding a cheap raw material for the preparation of the aerogel.
Drawings
FIG. 1: XRD (a) and SEM (b) of the fly ash;
FIG. 2: preparation of SiO by using fly ash as raw material2-Al2O3A process flow diagram of the composite aerogel;
FIG. 3: the synthesized SiO2-Al2O3XR of composite aerogelsA D map;
FIG. 4: the synthesized SiO2-Al2O3SEM images of composite aerogels (a) pH 2.7(b) pH 2.9(c) pH 3.1 and (d) TEM images;
FIG. 5: the synthesized SiO2-Al2O3Composite aerogel of (a) N2Adsorption-desorption diagram and (b) pore size distribution diagram;
FIG. 6: the synthesized SiO2-Al2O3XRD patterns of the composite aerogel after calcination at different temperatures.
The specific implementation mode is as follows:
raw material selection
The raw material is from fly ash of a certain power plant in Shanxi Taiyuan, the fly ash and sodium hydroxide are uniformly mixed, the mixture is calcined for 1h at 350 ℃ in a muffle furnace to obtain an alkali fusion mixture, the alkali fusion mixture and a hydrochloric acid solution are mixed and stirred, and solid-liquid separation is carried out to obtain a liquid phase containing silicon and aluminum. Wherein, XRD and SEM images of the fly ash are shown in figure 1, and the content of elements in the fly ash is shown in Table 1. The calculation shows that the sum of the contents of the silicon-aluminum oxides in the fly ash is more than 80 percent.
TABLE 1 fly ash content (wt%)
Example 1 (scheme FIG. 2)
(1) Uniformly mixing the fly ash and sodium hydroxide (the mass ratio is 1:0.8), placing the mixture in a muffle furnace, and calcining the mixture for 2 hours at 350 ℃.
(2) And (2) grinding the alkali-fusion mixture obtained in the step (1), adding 30ml of hydrochloric acid (5mol/L) and 40ml of deionized water into 5g of the alkali-fusion mixture, and stirring until the reaction is completed.
(3) And (3) filtering the mixed solution in the step (2) to obtain a solution containing silicon and aluminum.
(4) To the solution obtained in step (3), aqueous ammonia (0.25mol/L) was added, and the pH of the solution was controlled to 2.7.
(5) And (3) after the gel obtained in the step (4) is aged for 1 day, washing the gel with deionized water for 2 times.
(6) And (3) carrying out solvent replacement on the gel obtained in the step (5) by using absolute ethyl alcohol, and drying in an oven at 45 ℃ for 3h and 75 ℃ for 12 h.
Example 2 (scheme 2)
(1) Uniformly mixing the fly ash and sodium hydroxide (the mass ratio is 1:1), placing the mixture in a muffle furnace, and calcining the mixture for 1.5 hours at the temperature of 400 ℃.
(2) And (2) grinding the alkali-fusion mixture obtained in the step (1), adding 25ml of hydrochloric acid (5mol/L) and 30ml of deionized water into 6g of the alkali-fusion mixture, and stirring until the reaction is completed.
(3) And (3) filtering the mixed solution in the step (2) to obtain a solution containing silicon and aluminum.
(4) To the solution obtained in step (3), aqueous ammonia (0.35mol/L) was added, and the pH of the solution was controlled to 2.9.
(5) And (3) after aging the gel obtained in the step (4) for 2 days, washing the gel with deionized water for three times.
(6) And (3) carrying out solvent replacement on the gel obtained in the step (5) by using absolute ethyl alcohol, drying for 3h at the temperature of 45 ℃, drying for 12h at the temperature of 65 ℃ and drying for 12h at the temperature of 75 ℃ in an oven.
Example 3 (scheme FIG. 2)
(1) Uniformly mixing the fly ash and sodium hydroxide (the mass ratio is 1:1.2), placing the mixture in a muffle furnace, and calcining the mixture for 1 hour at 500 ℃.
(2) And (2) grinding the alkali-fusion mixture obtained in the step (1), taking 4g of the alkali-fusion mixture, adding 35ml of hydrochloric acid (5mol/L) and 35ml of deionized water, and stirring until the reaction is complete.
(3) And (3) filtering the mixed solution in the step (2) to obtain a solution containing silicon and aluminum.
(4) To the solution obtained in step (3), aqueous ammonia (0.5mol/L) was added, and the pH of the solution was controlled to 3.1.
(5) After aging the gel obtained in step (4) for 3 days, it was washed with deionized water 4 times.
(6) And (3) carrying out solvent replacement on the gel obtained in the step (5) by using absolute ethyl alcohol, drying for 3h at 45 ℃, 6h at 55 ℃, 12h at 65 ℃ and 12h at 75 ℃ in an oven.
Concrete experimental results
SiO prepared based on different pH values2-Al2O3The XRD pattern (fig. 3) of the composite aerogel shows that all samples show a distinct steamed bread peak at about 25 °, indicating that all samples are amorphous. The SEM image and TEM image (FIG. 4) show that all samples have rough surfaces, and a large number of nanoparticles and holes are observed, and the structure is in a three-dimensional network. In addition, N2The adsorption and desorption curve is a type IV curve (figure 5), which shows that the mesoporous solid is generated. The specific surface area of the sample reached a maximum of 897m at pH 2.82The pore diameter is mostly distributed between 3.5 nm and 5.2 nm. These all meet the typical characteristics of the aerogel reported in the literature, and show that the prepared product is SiO2-Al2O3And (3) compounding the aerogel.
From SiO2-Al2O3XRD patterns (figure 6) of the composite aerogel after being calcined at different temperatures show that when the calcination temperature is increased from 700 ℃ to 1000 ℃, the aerogel still keeps an amorphous structure, and only a small amount of crystalline silicon dioxide is generated after the composite aerogel is calcined at 1000 ℃, which indicates that the prepared SiO is2-Al2O3The composite aerogel can bear the high temperature of 900 ℃ and has better thermal stability.
Claims (4)
1. Preparation of SiO from fly ash2-Al2O3The method for compounding aerogel material is characterized in that under the condition of continuously stirring at room temperature, the SiO is obtained by adding ammonia water into a liquid phase containing silicon and aluminum, aging for a period of time, washing with deionized water, replacing solvent and drying under normal pressure2-Al2O3Compounding aerogel; SiO 22-Al2O3The composite aerogel synthesis steps are as follows:
(1) uniformly mixing the fly ash and a proper amount of sodium hydroxide, and calcining the mixture in a muffle furnace for a certain time to obtain an alkali fusion mixture;
(2) mixing and stirring the alkali fusion mixture and a hydrochloric acid solution, and performing solid-liquid separation to obtain a liquid phase containing silicon and aluminum;
(3) under the condition of stirring at room temperature, dropwise adding a proper amount of ammonia water into a liquid phase containing silicon and aluminum to obtain wet gel;
(4) aging the gel obtained in step (3) at room temperature for a period of time;
(5) washing the gel obtained in the step (4) with deionized water;
(6) the washed gel is subjected to solvent replacement by absolute ethyl alcohol, and then the wet gel after solvent replacement is dried in an oven to obtain SiO2-Al2O3Compounding aerogel; SiO 22-Al2O3The specific surface area of the composite aerogel reaches the maximum of 897m2The pore size is distributed between 3.5 nm and 5.2 nm;
in the step (1), the temperature of the muffle furnace is 350-500 ℃, and the temperature is kept for 1-2 h;
and (3) dropwise adding 0.25-0.5mol/L of ammonia water, and controlling the pH value of the solution to be 2.7-3.1.
2. The method for preparing SiO from fly ash as claimed in claim 12-Al2O3The method for compounding the aerogel material is characterized in that the liquid-solid ratio ml/g range of the hydrochloric acid 5mol/L and the alkali fusion mixture in the step (2) is as follows: 5-8.
3. The method for preparing SiO from fly ash as claimed in claim 12-Al2O3The method for compounding the aerogel material is characterized in that the gel in the step (4) needs to be aged for 1-3 days.
4. The method for preparing SiO from fly ash as claimed in claim 12-Al2O3The method for compounding the aerogel material is characterized in that in the step (6), absolute ethyl alcohol solvent is used for replacing for 2-4 times; drying wet gel in oven at 40-50 deg.C for 2-4 hr, drying at 50-65 deg.C for 5-10 hr, and drying at 65-70 deg.C for 10-14 hr.
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| Title |
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| 用废弃煤矸石制备高比表面积的SiO2-Al2O3二元复合气凝胶;刘博 等;《化学工报》;20170531;第68卷(第5期);第2096-2104页 * |
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