CN117088670A - Method for preparing silicon-aluminum composite aerogel material by taking nepheline as raw material - Google Patents
Method for preparing silicon-aluminum composite aerogel material by taking nepheline as raw material Download PDFInfo
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- CN117088670A CN117088670A CN202310783795.7A CN202310783795A CN117088670A CN 117088670 A CN117088670 A CN 117088670A CN 202310783795 A CN202310783795 A CN 202310783795A CN 117088670 A CN117088670 A CN 117088670A
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- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 title claims abstract description 64
- 239000004964 aerogel Substances 0.000 title claims abstract description 53
- 229910052664 nepheline Inorganic materials 0.000 title claims abstract description 47
- 239000010434 nepheline Substances 0.000 title claims abstract description 47
- 239000000463 material Substances 0.000 title claims abstract description 36
- 239000002131 composite material Substances 0.000 title claims abstract description 34
- 239000002994 raw material Substances 0.000 title claims abstract description 31
- 238000000034 method Methods 0.000 title claims abstract description 28
- 230000002378 acidificating effect Effects 0.000 claims abstract description 17
- 229910052782 aluminium Inorganic materials 0.000 claims abstract description 11
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000002253 acid Substances 0.000 claims abstract description 10
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 10
- 239000010703 silicon Substances 0.000 claims abstract description 10
- 239000007788 liquid Substances 0.000 claims abstract description 4
- 239000012535 impurity Substances 0.000 claims description 32
- 239000011521 glass Substances 0.000 claims description 28
- 239000000243 solution Substances 0.000 claims description 27
- 238000002791 soaking Methods 0.000 claims description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 23
- 239000011240 wet gel Substances 0.000 claims description 23
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 19
- 238000012986 modification Methods 0.000 claims description 19
- 230000004048 modification Effects 0.000 claims description 19
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 18
- 239000000843 powder Substances 0.000 claims description 18
- 239000002893 slag Substances 0.000 claims description 18
- -1 sodium-silicon-aluminum Chemical compound 0.000 claims description 18
- 238000002844 melting Methods 0.000 claims description 17
- 230000008018 melting Effects 0.000 claims description 17
- 238000001816 cooling Methods 0.000 claims description 16
- 239000000835 fiber Substances 0.000 claims description 16
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 14
- 238000002156 mixing Methods 0.000 claims description 14
- 238000000498 ball milling Methods 0.000 claims description 8
- 239000012299 nitrogen atmosphere Substances 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 7
- 238000001914 filtration Methods 0.000 claims description 7
- 238000007602 hot air drying Methods 0.000 claims description 7
- 238000007885 magnetic separation Methods 0.000 claims description 7
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 7
- DDFHBQSCUXNBSA-UHFFFAOYSA-N 5-(5-carboxythiophen-2-yl)thiophene-2-carboxylic acid Chemical compound S1C(C(=O)O)=CC=C1C1=CC=C(C(O)=O)S1 DDFHBQSCUXNBSA-UHFFFAOYSA-N 0.000 claims description 6
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 6
- 239000003513 alkali Substances 0.000 claims description 6
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 claims description 6
- 150000007522 mineralic acids Chemical class 0.000 claims description 6
- 229910052863 mullite Inorganic materials 0.000 claims description 6
- 239000002904 solvent Substances 0.000 claims description 6
- GOOHAUXETOMSMM-UHFFFAOYSA-N Propylene oxide Chemical compound CC1CO1 GOOHAUXETOMSMM-UHFFFAOYSA-N 0.000 claims description 5
- 238000001035 drying Methods 0.000 claims description 5
- 239000011259 mixed solution Substances 0.000 claims description 5
- 239000003607 modifier Substances 0.000 claims description 5
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 claims description 4
- 239000003365 glass fiber Substances 0.000 claims description 4
- 239000003795 chemical substances by application Substances 0.000 claims description 3
- 239000002516 radical scavenger Substances 0.000 claims description 3
- 238000012216 screening Methods 0.000 claims description 2
- 238000000926 separation method Methods 0.000 claims description 2
- 238000006467 substitution reaction Methods 0.000 claims 2
- 238000002360 preparation method Methods 0.000 abstract description 18
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 abstract description 9
- 238000009413 insulation Methods 0.000 abstract description 6
- 230000001105 regulatory effect Effects 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 230000007062 hydrolysis Effects 0.000 abstract description 2
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 2
- 238000011056 performance test Methods 0.000 abstract description 2
- 230000001988 toxicity Effects 0.000 abstract description 2
- 231100000419 toxicity Toxicity 0.000 abstract description 2
- 238000004321 preservation Methods 0.000 abstract 1
- 239000000203 mixture Substances 0.000 description 16
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 14
- 229910018072 Al 2 O 3 Inorganic materials 0.000 description 8
- 229910004298 SiO 2 Inorganic materials 0.000 description 7
- FFUAGWLWBBFQJT-UHFFFAOYSA-N hexamethyldisilazane Chemical compound C[Si](C)(C)N[Si](C)(C)C FFUAGWLWBBFQJT-UHFFFAOYSA-N 0.000 description 6
- 239000002245 particle Substances 0.000 description 6
- 238000003756 stirring Methods 0.000 description 6
- 238000004090 dissolution Methods 0.000 description 5
- UQEAIHBTYFGYIE-UHFFFAOYSA-N hexamethyldisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)C UQEAIHBTYFGYIE-UHFFFAOYSA-N 0.000 description 5
- 229910052751 metal Inorganic materials 0.000 description 5
- 239000002184 metal Substances 0.000 description 5
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 description 4
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 3
- 230000000052 comparative effect Effects 0.000 description 3
- 238000012360 testing method Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 2
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 2
- 239000003054 catalyst Substances 0.000 description 2
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical compound C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 2
- LIVNPJMFVYWSIS-UHFFFAOYSA-N silicon monoxide Chemical compound [Si-]#[O+] LIVNPJMFVYWSIS-UHFFFAOYSA-N 0.000 description 2
- 238000003980 solgel method Methods 0.000 description 2
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical group [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- 238000003723 Smelting Methods 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- AZDRQVAHHNSJOQ-UHFFFAOYSA-N alumane Chemical class [AlH3] AZDRQVAHHNSJOQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011218 binary composite Substances 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229910052791 calcium Inorganic materials 0.000 description 1
- 239000011575 calcium Substances 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000000499 gel Substances 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- 239000011810 insulating material Substances 0.000 description 1
- 239000012774 insulation material Substances 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910052749 magnesium Inorganic materials 0.000 description 1
- 239000011777 magnesium Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910017604 nitric acid Inorganic materials 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229910052814 silicon oxide Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 238000000352 supercritical drying Methods 0.000 description 1
- 230000009466 transformation Effects 0.000 description 1
- 239000005051 trimethylchlorosilane Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
- C04B30/02—Compositions for artificial stone, not containing binders containing fibrous materials
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B30/00—Compositions for artificial stone, not containing binders
-
- C—CHEMISTRY; METALLURGY
- C04—CEMENTS; CONCRETE; ARTIFICIAL STONE; CERAMICS; REFRACTORIES
- C04B—LIME, MAGNESIA; SLAG; CEMENTS; COMPOSITIONS THEREOF, e.g. MORTARS, CONCRETE OR LIKE BUILDING MATERIALS; ARTIFICIAL STONE; CERAMICS; REFRACTORIES; TREATMENT OF NATURAL STONE
- C04B2201/00—Mortars, concrete or artificial stone characterised by specific physical values
- C04B2201/30—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values
- C04B2201/32—Mortars, concrete or artificial stone characterised by specific physical values for heat transfer properties such as thermal insulation values, e.g. R-values for the thermal conductivity, e.g. K-factors
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Ceramic Engineering (AREA)
- Materials Engineering (AREA)
- Structural Engineering (AREA)
- Organic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
The invention provides a method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material, which uses nepheline as a raw material to replace an organic silicon source and an organic aluminum source which are expensive and have certain toxicity, and carries out certain process treatment on the nepheline in the preparation process, the acidic silicon-aluminum solution prepared by the nepheline raw material after treatment can be directly used as a silicon source and aluminum source mixed raw material liquid for preparing silicon-aluminum gel, the proportion of the silicon source and the aluminum source is not required to be regulated again, and acid is not required to be added again for catalytic hydrolysis, so that the preparation cost is reduced, the preparation period is relatively shortened, the prepared silicon-aluminum aerogel has better performance, and has good room temperature thermal conductivity as low as 0.032W/m ∙ K through a thermal insulation performance test, and wide application prospect in the field of heat preservation and insulation.
Description
Technical Field
The invention belongs to the technical field of preparation of aerogel nano materials, and particularly relates to a method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material.
Background
Aerogel is a novel high-performance nano heat-insulating material with a porous and network-shaped structure, and is widely applied to the heat-insulating fields such as pipeline heat insulation, electric core heat protection and the like at present. However, the silicon oxide aerogel can only resist 600 ℃ at most for a long time, the aluminum oxide aerogel material has better high temperature resistance, the aluminum oxide aerogel material can be used for a long time up to 800 ℃, the aluminum oxide aerogel is doped by multi-component collocation to inhibit the crystal form transformation of aluminum oxide at high temperature, the high temperature resistant temperature of the aluminum silicon composite aerogel is expected to be increased to 1000 ℃, the aluminum silicon binary composite aerogel has higher thermal stability and temperature resistance, and the application of the aerogel material in the high temperature field is expected to be promoted.
The conventional silicon-aluminum composite aerogel is usually prepared by using a sol-gel method and using organic silanol and organic aluminum salt as main raw materials through a supercritical drying method, and the prepared silicon-aluminum aerogel has good performance, but has high raw material cost and production cost, so that the material is limited in application and is only rarely applied to some military and aviation fields.
Whereas nepheline powder is a silicate containing aluminum and sodium, rich in SiO 2 And Al 2 O 3 According to statistics of SiO 2 And Al 2 O 3 The content can reach 80 percent, and is mainly applied to the field of ceramic preparation at present. Because the nepheline has rich silicon-aluminum content and lower cost, the nepheline can be considered as a raw material for preparing silicon-aluminum aerogel, can greatly reduce the preparation cost and has better application prospect. However, nepheline is extremely poorly dissolved in conventional water, alcohol and acid solutions, and also contains components such as calcium, magnesium and the like, which brings inconvenience to the application of nepheline. In addition, when aerogel is prepared from nepheline as a raw material, it is difficult to directly obtain relatively pure intermediate raw materials (aluminum source, silicon source, etc.) by a simple smelting process and a simple cleaning process, and the use of intermediate raw materials containing impurities may result in difficulty in forming sol. And the performance of the finally prepared silicon-aluminum aerogel is greatly influenced by raw materials (components, component concentration and the like) and process conditions (pH value, temperature and the like) when the silicon-aluminum aerogel is prepared, so that certain difficulty is brought to further preparing the silicon-aluminum aerogel by utilizing nepheline. Therefore, a process was developed to solve the above problems and to achieve a low cost preparation of silica alumina aerogel with better performance using nephelineHas important significance.
Disclosure of Invention
The invention takes nepheline as a raw material, prepares the silicon-aluminum aerogel by combining a sol-gel method with an atmospheric pressure drying technology, and aims to provide a method which has low raw material cost and simple process and is suitable for large-scale production of silicon-aluminum composite aerogel materials.
The invention provides a method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material, which comprises the following steps:
s1, adding alkali into nepheline powder subjected to crushing, screening and magnetic separation, mixing, ball milling, melting, cooling, remelting and water cooling to obtain sodium-silicon-aluminum glass slag containing impurities;
s2, dissolving the sodium-silicon-aluminum glass slag by using acid, and performing solid-liquid separation to obtain a mixed solution containing silicon and aluminum;
s3, filtering the mixed solution in the step S2 to obtain an acidic silicon-aluminum solution;
s4, dropwise adding a proton capturing agent into the acidic silicon-aluminum solution in the S3 to form silicon-aluminum sol;
s5, adding fibers into the silica-alumina sol in the S4, fully soaking, standing to obtain wet gel, and aging and removing impurities from the wet gel;
or S51, directly standing the silica-alumina sol in the S4 to obtain wet gel, and aging and removing impurities from the wet gel;
s6, sequentially performing solvent replacement, modifier modification and drying on the wet gel subjected to aging and impurity removal in the step S5 or the step S51 to obtain the silicon-aluminum composite aerogel material.
Ball milling is carried out in the step S1 to ensure that the particle size of nepheline powder is smaller than 200 meshes;
the alkali in the S1 is one or two of sodium carbonate or sodium hydroxide;
the mass ratio of nepheline powder to alkali in the S1 is 1:0.2 to 5; the melting temperatures in the step S1 are 900-1550 ℃ and the melting time is 30-150 min;
the S1 is performed with high-temperature melting after the cooling treatment, and then cold water is added for a period of time; the sodium-silicon-aluminum glass slag formed by the operation can be better dissolved in acid, and the subsequent operation is convenient.
The acid in the step S2 is inorganic acid, and the inorganic acid is one or a mixture of any two of hydrochloric acid, nitric acid and hydrofluoric acid;
the concentration of the inorganic acid is 0.5-5 mol/L, and the volume of the acid added into each 1kg of sodium-silicon-aluminum glass slag is 1-5L; the adding concentration and the adding amount of the acid are controlled, so that on one hand, the sodium-silicon-aluminum glass slag is fully dissolved, on the other hand, the acidic silicon-aluminum solution with proper concentration and acidity of a silicon source and an aluminum source is conveniently prepared, and the subsequent process for preparing the silicon-aluminum composite aerogel can be reduced.
The proton trapping agent is propylene oxide or ammonium fluoride dropwise added in the step S4; the dosage of the proton scavenger is 1-10wt% of the mass of the acidic silicon-aluminum solution.
And the fibers in the step S5 are one of glass fiber felt, aluminum silicate fiber felt and mullite fiber felt.
The fibers may also be staple fibers.
The aging and impurity removal in S5 or S51 are carried out by soaking wet gel in warm water for 2-4 h, and the temperature of the warm water is maintained to be 60 ℃ in the soaking process.
And the solvent replacement in the step S6 is carried out by soaking in ethanol for 3-5 h, and the temperature of the solvent replacement is 60 ℃.
And (3) in the step S6, the modification is carried out by soaking in a modifier for 2-4 h, and the modification temperature is 60 ℃.
And S6, drying by hot air at 90-160 ℃ in a nitrogen atmosphere.
The modifier in the S6 is one or more of hexamethyldisiloxane, hexamethyldisilazane or trimethylchlorosilane.
Compared with the prior art, the invention has the following beneficial effects:
(1) The nepheline has abundant reserves, low price and abundant silicon-aluminum content, and the invention uses nepheline as raw material to replace the organic silicon source and the organic aluminum source which are expensive and have certain toxicity, so that the preparation cost is lower;
(2) The method is used for carrying out treatment on nepheline in advance by a certain process, comprises the steps of carrying out simple impurity removal on the nepheline, then adding a proton scavenger to promote the formation of sol, so that silica-alumina sol can be better formed without thoroughly removing impurities, the prepared silica-alumina aerogel has better performance, and through a heat insulation performance test, the room temperature heat conductivity is as low as 0.032W/m.K, the high-temperature stability is good, and the method has wide application prospect in the heat insulation field;
(3) The preparation method is simple and operated, the solution prepared by the nepheline powder after treatment can be directly used as the silicon source and aluminum source mixed raw material liquid for preparing the silicon-aluminum gel, the proportion of the silicon source and the aluminum source is not required to be regulated again, and acid is not required to be added again for catalytic hydrolysis, so that the preparation period is relatively shortened.
Detailed Description
The following examples are intended to further illustrate the present invention but are not to be construed as limiting its scope, as many insubstantial modifications and adaptations of the invention that are within the scope of the invention as described above would be within the skill of the art.
Example 1
And (3) passing the crushed and screened nepheline powder through a mesh screen with the diameter of 1mm to remove larger impurities, and carrying out magnetic separation to further remove impurity metal impurities. Mixing 1000g of nepheline powder with 2500g of sodium carbonate, ball milling by adopting a ball mill to ensure that the particle size is smaller than 200 meshes, placing the mixture in a glass melting furnace to be melted at 1300 ℃ for 60min, naturally cooling the mixture to room temperature, and placing the mixture in the glass melting furnace to be melted at 1300 ℃ for 60min to prepare sodium-silicon-aluminum glass slag containing impurities. Pouring sodium-silicon-aluminum glass slag into 200ml of water for water cooling treatment, then adding 3L of hydrochloric acid (2 mol/L) for dissolution, and filtering to obtain an acidic silicon-aluminum solution;
directly dripping 1.2wt% of propylene oxide solution into the separated acidic silica-alumina solution, regulating the pH to 2.2 to obtain silica-alumina sol, mixing the silica-alumina sol with a glass fiber felt to fully impregnate the silica-alumina sol with the glass fiber felt, standing to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours; taking out, and soaking in 60 ℃ ethanol for 4 hours; and then, soaking the aluminum-silicon composite aerogel material in hexamethyldisilazane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification is finished to obtain the aluminum-silicon composite aerogel material.
Example 2
And (3) passing the crushed and screened nepheline powder through a mesh screen with the diameter of 1mm to remove larger impurities, and carrying out magnetic separation to further remove impurity metal impurities. Mixing 1000g of nepheline powder with 2500g of sodium carbonate, ball milling by adopting a ball mill to ensure that the particle size is smaller than 200 meshes, placing the mixture in a glass melting furnace to be melted at 1300 ℃ for 60min, naturally cooling the mixture to room temperature, and placing the mixture in the glass melting furnace to be melted at 1300 ℃ for 60min to prepare sodium-silicon-aluminum glass slag containing impurities. Pouring sodium-silicon-aluminum glass slag into 200ml of water for water cooling treatment, then adding 3L of hydrochloric acid (2 mol/L) for dissolution, and filtering to obtain an acidic silicon-aluminum solution;
directly dripping 2.5wt% of propylene oxide solution into the separated acidic silica-alumina solution, regulating the pH to 2.5 to obtain silica-alumina sol, mixing the silica-alumina sol with an aluminum silicate fiber felt to fully impregnate the aluminum silicate fiber felt into the silica-alumina sol, standing to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours; taking out, and soaking in 60 ℃ ethanol for 4 hours; and then soaking the aluminum silicon composite aerogel material in hexamethyldisiloxane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification is finished to obtain the aluminum silicon composite aerogel material.
Example 3
And (3) passing the crushed and screened nepheline powder through a mesh screen with the diameter of 1mm to remove larger impurities, and carrying out magnetic separation to further remove impurity metal impurities. Mixing 1000g of nepheline powder with 2500g of sodium carbonate, ball milling by adopting a ball mill to ensure that the particle size is smaller than 200 meshes, placing the mixture in a glass melting furnace to be melted at 1300 ℃ for 60min, naturally cooling the mixture to room temperature, and placing the mixture in the glass melting furnace to be melted at 1300 ℃ for 60min to prepare sodium-silicon-aluminum glass slag containing impurities. Pouring sodium-silicon-aluminum glass slag into 200ml of water for water cooling treatment, then adding 3L of hydrochloric acid (2 mol/L) for dissolution, and filtering to obtain an acidic silicon-aluminum solution;
directly dripping 1.7wt% propylene oxide solution into the separated acidic silica-alumina solution, regulating the pH to 2.4 to obtain silica-alumina sol, mixing the silica sol with mullite fiber felt to fully impregnate the mullite fiber felt into the silica-alumina sol, standing to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours; taking out, and soaking in 60 ℃ ethanol for 4 hours; and then soaking the aluminum silicon composite aerogel material in hexamethyldisiloxane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification is finished to obtain the aluminum silicon composite aerogel material.
Example 4
And (3) passing the crushed and screened nepheline powder through a mesh screen with the diameter of 1mm to remove larger impurities, and carrying out magnetic separation to further remove impurity metal impurities. Mixing 1000g of nepheline powder with 2500g of sodium carbonate, ball milling by adopting a ball mill to ensure that the particle size is smaller than 200 meshes, placing the mixture in a glass melting furnace to be melted at 1300 ℃ for 60min, naturally cooling the mixture to room temperature, and placing the mixture in the glass melting furnace to be melted at 1300 ℃ for 60min to prepare sodium-silicon-aluminum glass slag containing impurities. Pouring sodium-silicon-aluminum glass slag into 200ml of water for water cooling treatment, then adding 3L of hydrochloric acid (2 mol/L) for dissolution, and filtering to obtain an acidic silicon-aluminum solution;
directly dripping 10wt% ammonium fluoride solution (the mass concentration of the ammonium fluoride solution is 30%) into the separated acidic silicon-aluminum solution, directly standing the silicon-aluminum sol to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours; taking out, and soaking in 60 ℃ ethanol for 4 hours; and then soaking the aluminum silicon composite aerogel material in hexamethyldisiloxane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification is finished to obtain the aluminum silicon composite aerogel material.
Example 5
And (3) passing the crushed and screened nepheline powder through a mesh screen with the diameter of 1mm to remove larger impurities, and carrying out magnetic separation to further remove impurity metal impurities. Mixing 1000g of nepheline powder with 2500g of sodium carbonate, ball milling by adopting a ball mill to ensure that the particle size is smaller than 200 meshes, placing the mixture in a glass melting furnace to be melted at 1300 ℃ for 60min, naturally cooling the mixture to room temperature, and placing the mixture in the glass melting furnace to be melted at 1300 ℃ for 60min to prepare sodium-silicon-aluminum glass slag containing impurities. Pouring sodium-silicon-aluminum glass slag into 200ml of water for water cooling treatment, then adding 5L of hydrochloric acid (2 mol/L) for dissolution, and filtering to obtain an acidic silicon-aluminum solution;
directly dripping 5wt% ammonium fluoride solution (the mass concentration of the ammonium fluoride solution is 25%) into the separated acidic silicon-aluminum solution, directly standing the silica sol to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours; taking out, and soaking in 60 ℃ ethanol for 4 hours; and then soaking the aluminum silicon composite aerogel material in hexamethyldisiloxane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification is finished to obtain the aluminum silicon composite aerogel material.
Comparative example 1
(1)Al 2 O 3 Preparation of sol: according to n (ASB) to n (C) 2 H 5 OH)∶n(H 2 O) =1:16:1.2 mixing 246.32g ASB, 736g ethanol and 21.6g water, stirring at 60deg.C for 60min, gradually clarifying the solution from turbid, stopping stirring, sealing, standing, and naturally cooling to room temperature to obtain Al 2 O 3 Sol;
(2)SiO 2 preparation of sol: according to n (TEOS) to n (C) 2 H 5 OH)∶n(H 2 O) =1:4:1 measured 208.33g TEOS 184.28g C 2 H 5 OH、18g H 2 O, fully mixing with 0.001mol of hydrochloric acid, and continuously stirring the mixed solution for 60min to obtain SiO 2 Sol;
(3) Preparing a catalyst: 6ml glacial acetic acid, 43ml H 2 O and 50ml CH 3 Mixing OH uniformly, and stirring for 5min;
(4) Preparation of SiO 2 -Al 2 O 3 Sol: taking Al in (1) according to the mole ratio of Al to Si of 1:1 2 O 3 Sol and SiO in (2) 2 Mixing the sol, stirring, adding 20ml of catalyst solution, and stirring for 10min to obtain Al 2 O 3 -SiO 2 Sol;
(5) SiO is then added with 2 -Al 2 O 3 The sol is compounded with the mullite fiber felt to enable the mullite fiber felt to fully impregnate SiO 2 -Al 2 O 3 Sol, standing to obtain wet gel, and soaking the wet gel in hot water at 60 ℃ for 3 hours;
(6) And (3) taking out, soaking in ethanol at 60 ℃ for 4 hours, then soaking in hexamethyldisilazane at 60 ℃ for 3 hours for modification, and carrying out hot air drying in a nitrogen atmosphere at 120 ℃ after modification to obtain the silicon-aluminum composite aerogel material.
Test results
| Test item | Coefficient of thermal conductivity (W/m.K, 25 ℃ C.) | Use temperature (. Degree. C.) | Raw material cost (Yuan/m) 2 ) | Preparation period (Tian) |
| Example 1 | 0.035 | 800 | 70 | 3 |
| Example 2 | 0.038 | 1050 | 90 | 3 |
| Example 3 | 0.035 | 1100 | 110 | 3 |
| Example 4 | 0.032 | 1000 | 300 | 3 |
| Example 5 | 0.033 | 1000 | 260 | 3 |
| Comparative example 1 | 0.028 | 1100 | 360 | 4 |
The embodiment adopts nepheline powder as a raw material, and adopts the preparation method provided by the invention to prepare the silicon-aluminum composite aerogel material, and the comparative example adopts the method disclosed in the prior art to prepare the silicon-aluminum aerogel material. As can be seen from the test results, the silicon-aluminum composite aerogel material prepared by the preparation method has better heat insulation performance than the traditional heat insulation material, lower preparation cost, shorter preparation period and excellent high temperature resistance.
Claims (10)
1. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material is characterized by comprising the following steps of:
s1, adding alkali into nepheline powder subjected to crushing, screening and magnetic separation, mixing, ball milling, melting, cooling, remelting and water cooling to obtain sodium-silicon-aluminum glass slag containing impurities;
s2, dissolving the sodium-silicon-aluminum glass slag by using acid, and performing solid-liquid separation to obtain a mixed solution containing silicon and aluminum;
s3, filtering the mixed solution in the step S2 to obtain an acidic silicon-aluminum solution;
s4, dropwise adding a proton capturing agent into the acidic silicon-aluminum solution in the S3 to form silicon-aluminum sol;
s5, adding fibers into the silica-alumina sol in the S4, fully soaking, standing to obtain wet gel, and aging and removing impurities from the wet gel;
or S51, directly standing the silica-alumina sol in the S4 to obtain wet gel, and aging and removing impurities from the wet gel;
s6, sequentially performing solvent replacement, modifier modification and drying on the wet gel subjected to aging and impurity removal in the step S5 or the step S51 to obtain the silicon-aluminum composite aerogel material.
2. The method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the alkali in the S1 is one or two of sodium carbonate or sodium hydroxide.
3. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the melting temperature in the step S1 is 900-1550 ℃ and the melting time is 30-150 min.
4. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the mass ratio of nepheline powder to alkali in S1 is 1: 0.2-5.
5. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material, according to claim 1, wherein the acid in the S2 is inorganic acid, the concentration of the inorganic acid is 0.5-5 mol/L, and the volume of the inorganic acid added into each 1kg of sodium-silicon-aluminum glass slag is 1-5L.
6. The method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the proton scavenger in the step S4 is propylene oxide or ammonium fluoride.
7. The method for preparing a silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the fiber in the step S5 is one of a glass fiber felt, an aluminum silicate fiber felt and a mullite fiber felt.
8. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the solvent substitution in the step S6 is performed by soaking in ethanol for 3-5 hours, and the temperature of the solvent substitution is 60 ℃.
9. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the modification in the step S6 is carried out by soaking in a modifier for 2-4 hours, and the modification temperature is 60 ℃.
10. The method for preparing the silicon-aluminum composite aerogel material by taking nepheline as a raw material according to claim 1, wherein the drying in the step S6 is hot air drying at 90-160 ℃ in a nitrogen atmosphere.
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