CN112340744A - Preparation method of silicon-aluminum composite aerogel - Google Patents
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 54
- 239000002131 composite material Substances 0.000 title claims abstract description 36
- 239000004964 aerogel Substances 0.000 title claims abstract description 25
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 238000002156 mixing Methods 0.000 claims abstract description 35
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 32
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 32
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 30
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 25
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 25
- 239000010881 fly ash Substances 0.000 claims abstract description 25
- 238000001035 drying Methods 0.000 claims abstract description 17
- 229910000323 aluminium silicate Inorganic materials 0.000 claims abstract description 16
- HNPSIPDUKPIQMN-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Al]O[Al]=O HNPSIPDUKPIQMN-UHFFFAOYSA-N 0.000 claims abstract description 16
- 239000003513 alkali Substances 0.000 claims abstract description 15
- 150000001768 cations Chemical class 0.000 claims abstract description 14
- 239000011347 resin Substances 0.000 claims abstract description 14
- 229920005989 resin Polymers 0.000 claims abstract description 14
- 238000009835 boiling Methods 0.000 claims abstract description 13
- 239000003054 catalyst Substances 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 10
- 238000000967 suction filtration Methods 0.000 claims abstract description 10
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000002738 chelating agent Substances 0.000 claims abstract description 7
- 239000012295 chemical reaction liquid Substances 0.000 claims abstract description 7
- 239000000706 filtrate Substances 0.000 claims abstract description 7
- 230000032683 aging Effects 0.000 claims abstract description 3
- 238000001354 calcination Methods 0.000 claims description 21
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical group [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 15
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 15
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 12
- YRKCREAYFQTBPV-UHFFFAOYSA-N acetylacetone Chemical compound CC(=O)CC(C)=O YRKCREAYFQTBPV-UHFFFAOYSA-N 0.000 claims description 12
- 238000006243 chemical reaction Methods 0.000 claims description 10
- 230000002431 foraging effect Effects 0.000 claims description 9
- 238000005406 washing Methods 0.000 claims description 9
- SMZOGRDCAXLAAR-UHFFFAOYSA-N aluminium isopropoxide Chemical group [Al+3].CC(C)[O-].CC(C)[O-].CC(C)[O-] SMZOGRDCAXLAAR-UHFFFAOYSA-N 0.000 claims description 8
- XYIBRDXRRQCHLP-UHFFFAOYSA-N ethyl acetoacetate Chemical group CCOC(=O)CC(C)=O XYIBRDXRRQCHLP-UHFFFAOYSA-N 0.000 claims description 6
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- 238000004519 manufacturing process Methods 0.000 claims description 4
- WOZZOSDBXABUFO-UHFFFAOYSA-N tri(butan-2-yloxy)alumane Chemical compound [Al+3].CCC(C)[O-].CCC(C)[O-].CCC(C)[O-] WOZZOSDBXABUFO-UHFFFAOYSA-N 0.000 claims description 4
- 239000000203 mixture Substances 0.000 claims description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims 2
- 229910021529 ammonia Inorganic materials 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 4
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 abstract description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 abstract description 2
- 238000013329 compounding Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 239000010883 coal ash Substances 0.000 description 4
- JEGUKCSWCFPDGT-UHFFFAOYSA-N h2o hydrate Chemical compound O.O JEGUKCSWCFPDGT-UHFFFAOYSA-N 0.000 description 4
- 238000003837 high-temperature calcination Methods 0.000 description 4
- 239000000843 powder Substances 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- 238000012216 screening Methods 0.000 description 4
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- -1 polysiloxane Polymers 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000011343 solid material Substances 0.000 description 2
- 238000006467 substitution reaction Methods 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 235000019353 potassium silicate Nutrition 0.000 description 1
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
Classifications
-
- 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
- C01B33/20—Silicates
- C01B33/26—Aluminium-containing silicates, i.e. silico-aluminates
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/10—Solid density
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention belongs to the technical field of materials, and relates to a preparation method of a silicon-aluminum composite aerogel. The method comprises the following steps: 1. pretreating fly ash; 2. mixing the pretreated fly ash with a hydrochloric acid solution, carrying out suction filtration on the obtained reaction liquid after boiling water bath, mixing the obtained filter residue with an alkali solution, and carrying out suction filtration to obtain an aluminosilicate solution; 3. performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silica-alumina sol; 4. preparing pure aluminum sol: mixing aluminum salt and a chelating agent, and dropwise adding ethanol, water and a catalyst to react to obtain pure aluminum sol; 5. uniformly mixing the silicon-aluminum sol prepared in the step (3) and the pure aluminum sol obtained in the step (4) to prepare silicon-aluminum composite sol; 6. and standing, aging and drying the silicon-aluminum composite sol to obtain the silicon-aluminum composite sol. The silicon-aluminum composite aerogel prepared by utilizing the fly ash has high porosity and specific surface area, and has the quality similar to that of gel obtained by compounding pure silica sol and pure aluminum sol.
Description
Technical Field
The invention belongs to the technical field of materials, and relates to a preparation method of a silicon-aluminum composite aerogel.
Background
Aerogel is the most ideal light heat-insulating material at present, is a light, amorphous and porous solid material composed of nano colloidal particles or high polymer molecules, and has extremely low density, high specific surface area and high porosity. The pore size of the aerogel (< 50nm) is smaller than the mean free path of air molecules (about 70 nm), there is no air convection inside the pores of the aerogel, and thus there is extremely low gaseous heat conduction; meanwhile, the aerogel has extremely high porosity and low volume ratio of solid, so that the solid heat conduction is also very low, so that the aerogel has extremely low heat conductivity and is considered to be the solid material which is found to have the best heat insulation performance at present.
The SiO can be prepared by selecting metal organic matters as raw materials by a sol-gel method and performing supercritical drying2An aerogel. However, the raw materials needed to be used at present, such as tetraethyl orthosilicate E-40 polysiloxane polyoxysiloxane water glass alkaline silica sol, are expensive, and the large-scale commercial production and application of aerogel materials are restricted by the high toxicity of part of the raw materials, the complex supercritical drying technology adopted, the high cost of equipment and the high risk. Therefore, the search for cheap, efficient and environment-friendly raw materials has become a necessary trend of current aerogel material research with great necessity and practical significance.
Disclosure of Invention
The invention mainly aims to provide a method for preparing silicon-aluminum composite aerogel by efficiently utilizing fly ash.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of silicon-aluminum composite aerogel comprises the following steps:
step 1, pretreating fly ash;
step 2, mixing the pretreated fly ash with a hydrochloric acid solution, carrying out suction filtration on the obtained reaction liquid after boiling water bath, mixing the obtained filter residue with an alkali solution, and carrying out suction filtration to obtain an aluminosilicate solution;
step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol;
step 4, preparing pure aluminum sol: mixing aluminum salt and a chelating agent, and dropwise adding ethanol, water and a catalyst to react to obtain pure aluminum sol;
step 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 to prepare silicon-aluminum composite sol;
and 6, standing, aging and drying the silicon-aluminum composite sol to obtain the silicon-aluminum composite sol.
Preferably, in step 1, the mass ratio of fly ash to sodium carbonate is 1: 1-5, calcining at high temperature, washing with water, and drying.
Further preferably, the calcination temperature is 500-800 ℃, the calcination time is 1-3h, and the drying time is 1-3h under the temperature of 150-200 ℃ after 3 times of water washing.
Preferably, in the step 2, the fly ash and the hydrochloric acid solution are mixed according to the mass volume ratio of 1:5-10g/mL, and the mixture is reacted in a boiling water bath for 1-3 h; mixing the obtained filter residue and an alkali solution according to the mass-volume ratio of 1:5-10g/mL, and reacting for 1-3 h.
Further preferably, the concentration of the hydrochloric acid solution is 3-5mol/L, and the concentration of the alkali solution is 15-30 g/L.
Preferably, in step 3, the aluminosilicate solution is subjected to cation resin exchange until the pH value of the solution is 2-3, the catalyst used is ammonia water, and the reaction pH value of the solution is 5-7.
Preferably, in step 4, the molar ratio of the aluminum salt, the chelating agent, the ethanol, the water and the catalyst is: 1:0.1-0.5:5-20:1-3: 0.1-1;
further preferably, the aluminum salt is aluminum isopropoxide or aluminum sec-butoxide; the chelating agent is ethyl acetoacetate or acetylacetone; the catalyst is ammonia water.
Preferably, in the step 5, the mass ratio of the silicon-aluminum sol to the pure aluminum sol is 5-10: 1.
Preferably, in the step 6, the silicon-aluminum composite sol is kept stand for 1 to 3 hours at the temperature of between 60 and 85 ℃, and an alcohol solvent for aging is added for aging for 24 to 48 hours.
Compared with the prior art, the invention has the following advantages:
the method of the invention effectively pretreats the fly ash, fully activates the fly ash, and can remove a large amount of impurities existing in the original fly ash after the exchange of the cation resin, thereby improving the sol quality.
The silicon-aluminum composite aerogel prepared by utilizing the fly ash has high porosity and specific surface area, and has the quality similar to that of gel obtained by compounding pure silica sol and pure aluminum sol. The invention realizes the high-efficiency resource utilization of the fly ash and reduces the production cost of enterprises.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the invention as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of the stated features, steps, operations, and/or combinations thereof, unless the context clearly indicates otherwise.
In order to make the technical solutions of the present invention more clearly understood by those skilled in the art, the technical solutions of the present invention will be described in detail below with reference to specific embodiments.
Example 1 preparation method of silicon-aluminum composite aerogel
The method comprises the following steps:
step 1, coal ash pretreatment: mixing fly ash and sodium carbonate according to the mass ratio of 1:1, and then carrying out high-temperature calcination, water washing and drying. The calcining temperature is 500 ℃, the calcining time is 3 hours, and the calcining temperature is 3 times, and the calcining time is 1 hour after the calcining time is 3 times and the calcining time is 150 ℃.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:5g/mL, and reacting in a boiling water bath for 3 hours; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:5g/mL for reaction for 3 h. The concentration of the hydrochloric acid solution is 3mol/L, and the concentration of the alkali solution is 15 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum isopropoxide and ethyl acetoacetate, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of aluminum isopropoxide to ethyl acetoacetate to ethanol to water to ammonia water is as follows: 1:0.1:5:1:0.1.
And 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to the mass ratio of 5:1 to prepare the silicon-aluminum composite sol.
And 6, standing the silicon-aluminum composite sol for 1h at 60 ℃, adding an alcohol solvent for aging for 24h, and finally drying the silicon-aluminum gel in a drying oven at 110 ℃ for 24h under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.167g/cm3The porosity was 94.4%, and the specific surface area was 691.7m2/g。
Example 2 preparation method of silicon-aluminum composite aerogel
The method comprises the following steps:
step 1, coal ash pretreatment: mixing the fly ash and sodium carbonate according to the mass ratio of 1:5, and then carrying out high-temperature calcination, washing and drying. Calcining at 800 deg.C for 1 hr, washing with water for 3 times, and drying at 200 deg.C for 1 hr.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:10g/mL, and reacting in a boiling water bath for 1 h; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:10g/mL for reaction for 1 h. The concentration of the hydrochloric acid solution is 5mol/L, and the concentration of the alkali solution is 30 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum isopropoxide and ethyl acetoacetate, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of aluminum isopropoxide to ethyl acetoacetate to ethanol to water to ammonia water is as follows: 1: 0.5: 20:3: 1;
and 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to the mass ratio of 10:1 to prepare the silicon-aluminum composite sol.
Step 6, standing the silicon-aluminum composite sol at 85 ℃ for 1h, adding an alcohol solvent for agingAging was carried out for 48 h. Finally, the silicon-aluminum gel is placed in a drying oven at 110 ℃ and dried for 24 hours under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.156g/cm3The porosity was 95.3%, and the specific surface area was 679.9m2/g。
Example 3 preparation method of silicon-aluminum composite aerogel
The method comprises the following steps:
step 1, coal ash pretreatment: mixing the fly ash and sodium carbonate according to the mass ratio of 1:3, and then carrying out high-temperature calcination, washing and drying. The calcining temperature is 700 ℃, the calcining time is 1.5h, and the calcining temperature is 3 times, and the calcining time is 2h under 175 ℃.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:8g/mL, and reacting in a boiling water bath for 1.5 h; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:8g/mL for reaction for 2 h. The concentration of the hydrochloric acid solution is 3.5mol/L, and the concentration of the alkali solution is 20 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum isopropoxide and acetylacetone, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of aluminum isopropoxide to acetylacetone to ethanol to water to ammonia water is as follows: 1:0.3:10:2: 0.5;
and 5, mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to a mass ratio of 8: 1, uniformly mixing to prepare silicon-aluminum composite sol;
and 6, standing the silicon-aluminum composite sol at 80 ℃ for 1-3h, and adding an alcohol solvent for aging for 24-48h for aging. Finally, the silicon-aluminum gel is placed in a drying oven at 110 ℃ and dried for 24 hours under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.172g/cm3The porosity was 96, 23%, and the specific surface area was 681.6m2/g。
Example 4 preparation method of silicon-aluminum composite aerogel
The method comprises the following steps:
step 1, coal ash pretreatment: mixing the fly ash and sodium carbonate according to the mass ratio of 1:3, and then carrying out high-temperature calcination, washing and drying. The calcining temperature is 700 ℃, the calcining time is 1.5h, and the calcining temperature is 3 times, and the calcining time is 2h under 175 ℃.
Step 2, mixing the pretreated fly ash and a hydrochloric acid solution according to the mass volume ratio of 1:8g/mL, and reacting in a boiling water bath for 1.5 h; and after boiling water bath, carrying out suction filtration on the obtained reaction liquid, and mixing the obtained filter residue and the alkali solution according to the mass-volume ratio of 1:8g/mL for reaction for 2 h. The concentration of the hydrochloric acid solution is 3.5mol/L, and the concentration of the alkali solution is 20 g/L.
Step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol; in step 3, cation resin exchange is carried out on the aluminosilicate solution until the pH value of the solution is 2-3, the used catalyst is ammonia water, and the pH value of the solution reaction is 5-7.
Step 4, preparing pure aluminum sol: mixing aluminum sec-butoxide with acetylacetone, and dropwise adding ethanol, water and ammonia water to react to obtain pure aluminum sol; the molar ratio of the aluminum sec-butoxide to the acetylacetone to the ethanol to the water to the ammonia water is as follows: 1:0.3:10:2: 0.5;
step 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 according to the mass ratio of 6:1 to prepare silicon-aluminum composite sol;
and 6, standing the silicon-aluminum composite sol at 80 ℃ for 1-3h, and adding an alcohol solvent for aging for 24-48h for aging. Finally, the silica-alumina gel is placed in a drying oven at 105 ℃ and dried for 24 hours under normal pressure. The silicon-aluminum composite aerogel powder obtained by crushing and screening has the density of 0.163g/cm3The porosity was 96.17%, and the specific surface area was 679.3m2/g。
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. The preparation method of the silicon-aluminum composite aerogel is characterized by comprising the following steps:
step 1, pretreating fly ash;
step 2, mixing the pretreated fly ash with a hydrochloric acid solution, carrying out suction filtration on the obtained reaction liquid after boiling water bath, mixing the obtained filter residue with an alkali solution, and carrying out suction filtration to obtain an aluminosilicate solution;
step 3, performing cation resin exchange on the aluminosilicate solution obtained in the step 2, and catalyzing the obtained filtrate to obtain silicon-aluminum sol;
step 4, preparing pure aluminum sol: mixing aluminum salt and a chelating agent, and dropwise adding ethanol, water and a catalyst to react to obtain pure aluminum sol;
step 5, uniformly mixing the silicon-aluminum sol prepared in the step 3 and the pure aluminum sol obtained in the step 4 to prepare silicon-aluminum composite sol;
and 6, standing, aging and drying the silicon-aluminum composite sol to obtain the silicon-aluminum composite sol.
2. The preparation method according to claim 1, wherein in the step 1, the fly ash and the sodium carbonate are mixed according to a mass ratio of 1: 1-5, calcining at high temperature, washing with water, and drying.
3. The method as claimed in claim 2, wherein the calcination temperature is 500-800 ℃, the calcination time is 1-3h, and the washing with water 3 times is 150-200 ℃ and the drying time is 1-3 h.
4. The preparation method of claim 1, wherein in the step 2, the fly ash and the hydrochloric acid solution are mixed according to the mass volume ratio of 1:5-10g/mL, and the mixture is reacted in a boiling water bath for 1-3 h; mixing the obtained filter residue and an alkali solution according to the mass-volume ratio of 1:5-10g/mL, and reacting for 1-3 h.
5. The production method according to claim 4, wherein the hydrochloric acid solution has a concentration of 3 to 5mol/L and the alkali solution has a concentration of 15 to 30 g/L.
6. The process according to claim 1, wherein in step 3, the aluminosilicate solution is subjected to cation resin exchange to a pH 2 to 3 around the solution, the catalyst used is ammonia, and the solution has a reaction pH of 5 to 7.
7. The method according to claim 1, wherein in step 4, the molar ratio of the aluminum salt, the chelating agent, the ethanol, the water and the catalyst is: 1:0.1-0.5:5-20:1-3:0.1-1.
8. The production method according to claim 7, wherein the aluminum salt is aluminum isopropoxide or aluminum sec-butoxide; the chelating agent is ethyl acetoacetate or acetylacetone; the catalyst is ammonia water.
9. The preparation method according to claim 1, wherein in the step 5, the mass ratio of the silicon-aluminum sol to the pure aluminum sol is 5-10: 1.
10. The preparation method according to claim 1, wherein in the step 6, the silicon-aluminum composite sol is left to stand at 60 to 85 ℃ for 1 to 3 hours, and an alcohol solvent for aging is added for aging for 24 to 48 hours.
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| CN115591517A (en) * | 2022-09-19 | 2023-01-13 | 山东科技大学（Cn） | Rice hull ash/fly ash-based adsorbent, preparation method and application thereof |
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| CN115591517B (en) * | 2022-09-19 | 2024-02-02 | 山东科技大学 | Rice hull ash/fly ash-based adsorbent, preparation method and application thereof |
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