CN117069428A - High-temperature-resistant high-strength aerogel material and preparation method thereof - Google Patents
High-temperature-resistant high-strength aerogel material and preparation method thereof Download PDFInfo
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- 239000004964 aerogel Substances 0.000 title claims abstract description 102
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
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- 239000000835 fiber Substances 0.000 claims abstract description 85
- 239000011259 mixed solution Substances 0.000 claims abstract description 85
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims abstract description 79
- 239000011858 nanopowder Substances 0.000 claims abstract description 41
- 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 abstract description 37
- 238000010438 heat treatment Methods 0.000 claims abstract description 37
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- 238000002156 mixing Methods 0.000 claims abstract description 29
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 27
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- 239000002127 nanobelt Substances 0.000 claims abstract description 13
- TWNQGVIAIRXVLR-UHFFFAOYSA-N oxo(oxoalumanyloxy)alumane Chemical compound O=[Al]O[Al]=O TWNQGVIAIRXVLR-UHFFFAOYSA-N 0.000 claims description 12
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 9
- 238000000034 method Methods 0.000 abstract description 32
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- 229920002748 Basalt fiber Polymers 0.000 description 3
- 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 description 3
- 229910052863 mullite Inorganic materials 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 239000011148 porous material Substances 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
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- C04B28/00—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements
- C04B28/005—Compositions of mortars, concrete or artificial stone, containing inorganic binders or the reaction product of an inorganic and an organic binder, e.g. polycarboxylate cements containing gelatineous or gel forming binders, e.g. gelatineous Al(OH)3, sol-gel binders
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- C04B38/00—Porous mortars, concrete, artificial stone or ceramic ware; Preparation thereof
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Abstract
The invention relates to a high-temperature-resistant high-strength aerogel material and a preparation method thereof, wherein the method comprises the following steps: uniformly mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water to obtain a mixed solution, and then placing the mixed solution at 150-300 ℃ for hydrothermal reaction to obtain gel; soaking the gel in water; drying the soaked soaking gel at normal pressure to obtain an aerogel material; and performing heat treatment on the aerogel material to obtain the high-temperature-resistant high-strength aerogel material. The high-temperature-resistant high-strength aerogel material prepared by the method is a cage-shaped nano structure surrounded by nano belts, has better mechanical strength, does not need a supercritical drying process, and can be directly obtained through normal-pressure drying and relatively low-temperature heat treatment steps.
Description
Technical Field
The invention relates to the technical field of aerogel preparation, in particular to a high-temperature-resistant high-strength aerogel material and a preparation method thereof.
Background
The nano porous aerogel (aerogel for short) material is a gel material with a dispersion medium as gas, and is a nano porous solid material with a network structure, which is formed by mutually accumulating colloid particles or high polymer molecules, wherein the size of pores in the material is in the order of nanometers. The porosity can reach 80-99.8%, the typical size of the holes is 1-100 nm, and the density can reach 3kg/m 3 The heat conductivity coefficient at room temperature is low. Because of the characteristics, the aerogel material has wide application potential in thermal, acoustic, optical, microelectronic and particle detection aspects. Currently, the most widely used field of aerogel is still the heat insulation field, and the unique nano structure of aerogel can effectively reduce convection conduction, solid phase conduction and heat radiation.
Most of the traditional aerogel materials are in pearl necklace-like structures formed by stacking nano particles, and in the drying process, the supercritical drying process is often needed, so that the preparation period and the preparation cost are greatly increased. In addition, aerogel materials of such structures exhibit brittleness and require structural reinforcement for practical use. However, the prior art structure strengthening process will bring about an increase in density, an increase in solid phase thermal conductivity, and an increase in process complexity, etc. In addition, there are some methods for preparing aerogel materials with strong frameworks, which have good structural strength, however, the method often needs a complicated high-temperature sintering process to increase the framework size to improve the strength of the materials, so that the new problems of high thermal conductivity, high brittleness and the like are brought. With the development of technology, higher requirements are put on the strength, the temperature resistance, the light weight and/or the heat insulation performance of aerogel heat insulation materials in various fields.
In summary, it is very necessary to provide a high-temperature-resistant high-strength aerogel material and a preparation method thereof.
Disclosure of Invention
In order to solve one or more technical problems in the prior art, the invention provides a high-temperature-resistant high-strength aerogel material and a preparation method thereof.
The invention provides a preparation method of a high-temperature-resistant high-strength aerogel material in a first aspect, which comprises the following steps:
(1) Uniformly mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water to obtain a mixed solution, and then placing the mixed solution at 150-300 ℃ for hydrothermal reaction to obtain gel;
(2) Soaking the gel in water to obtain a soaked gel;
(3) Drying the soaking treatment gel obtained in the step (2) at normal pressure to obtain an aerogel material;
(4) And (3) performing heat treatment on the aerogel material obtained in the step (3) to obtain the high-temperature-resistant high-strength aerogel material.
Preferably, the mass fraction of the alumina nano powder contained in the mixed solution is 5-20%.
Preferably, the mixed solution contains 1-15% of the sum of the mass fractions of the aluminum silicate fiber and the aluminum oxide fiber.
Preferably, the mass ratio of the aluminum silicate fiber to the aluminum oxide fiber is (1-3): 1, preferably 2:1.
Preferably, the hydrothermal reaction time is 1 to 48 hours, preferably 3 to 12 hours; and/or the soaking time is 6-72 h.
Preferably, the temperature of the normal pressure drying is 25-80 ℃, and the time of the normal pressure drying is 12-120 h.
Preferably, the temperature of the heat treatment is 600-1000 ℃, and the time of the heat treatment is 0.5-2 h.
Preferably, the concentration of the hydrochloric acid is 0.1-5 mol/L; and/or the dosage of the hydrochloric acid accounts for 0.3-5% of the total mass of the mixed solution.
Preferably, the high temperature resistant high strength aerogel material has a nanoribbon surrounding cage structure.
The present invention provides in a second aspect, high temperature resistant, high strength aerogel materials made by the method of the present invention described in the first aspect.
Compared with the prior art, the invention has at least the following beneficial effects:
(1) Compared with the traditional pearl necklace aerogel material, the high-temperature-resistant high-strength aerogel material prepared by the invention is a cage-shaped nano structure surrounded by a nano belt, has the porosity of about 95%, has the characteristics of ultra-light weight, has the heat-resistant temperature of more than 1200 ℃, and has better mechanical strength.
(2) The method adopts the water phase as a reaction medium, does not need a supercritical drying process and a relatively high-temperature heat treatment process or a complex step-by-step heat treatment process, avoids environmental pollution and waste caused by using an organic solvent in the preparation process, and can directly obtain the high-temperature-resistant high-strength aerogel material through normal-pressure drying and a relatively low-temperature heat treatment step after the gel is soaked in the water.
(3) The gel process in the preparation method is a hydrothermal process, is different from the traditional RTM (resin transfer molding) pressurizing and injecting glue process, is not limited by the shape and the size of the reinforcement body, and can be used for preparing aerogel materials with any shape and thickness.
(4) The density of the high-temperature-resistant high-strength aerogel material prepared by the invention can be as low as 0.2g/cm 3 About, compared with other aerogel materials with the same strength, the aerogel material has the characteristic of ultralow density; the aerogel material prepared by the method has excellent high temperature resistance on the premise of keeping low heat conductivity, and can realize heat insulation application at 1200 ℃ for a long time; the high-temperature-resistant high-strength aerogel material has the advantages of good temperature resistance, high strength, low density and good heat insulation performance.
Drawings
FIG. 1 is a flow chart of the preparation of the present invention.
FIG. 2 is an SEM image of a high temperature resistant and strong aerogel material prepared according to example 1 of the invention.
FIG. 3 is a macroscopic optical photograph of the high temperature resistant high strength aerogel material prepared in example 1 of the present invention; in the figure: (a) A macroscopic photomicrograph heat treated at 600℃for 1 hour in example 1; (b) The high temperature resistant high strength aerogel material prepared in example 1 was subjected to a heat treatment at 1200 ℃ for 2 hours.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the technical solutions of the present invention will be clearly and completely described below in connection with the embodiments of the present invention. It will be apparent that the described embodiments are some, but not all, embodiments of the invention. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The present invention provides, in a first aspect, a method for preparing a high temperature resistant high strength aerogel material, where the preparation flow chart is shown in fig. 1, and the method includes the following steps:
(1) Uniformly mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water to obtain a mixed solution, and then placing the mixed solution at 150-300 ℃ for hydrothermal reaction to obtain gel; in some more preferred embodiments, the temperature of the hydrothermal reaction is 200 to 300 ℃;
(2) Soaking the gel in water to obtain a soaked gel; according to the invention, the gel is soaked in water for aging, the water has good diffusivity and uniformity, the water can uniformly permeate into the gel, so that the aging process is more uniform, the water soaking aging can provide uniform wetting conditions, the uniform progress of internal reaction of the gel is facilitated, a finer pore structure is facilitated to be formed, cracks and defects of the finally formed aerogel are reduced, a higher specific surface area is provided, the soaking aging process can enhance the uniformity and connectivity of gel materials, and the aging in the water is facilitated to form a more stable gel structure, so that the subsequent normal-pressure drying process is facilitated;
(3) Drying the soaking treatment gel obtained in the step (2) at normal pressure to obtain an aerogel material;
(4) Performing heat treatment on the aerogel material obtained in the step (3) to obtain a high-temperature-resistant high-strength aerogel material; the heat treatment is performed under an air atmosphere.
The invention discovers that a mixed solution containing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid is subjected to a hydrothermal reaction, and in the hydrothermal process, the alumina silicate fiber and the alumina fiber can participate in the reaction, so that the alumina nano powder can form interaction with the alumina silicate fiber and the alumina fiber, and the interaction can lead the alumina nano powder to cross-link, cross-connect or wrap with the alumina silicate fiber and the alumina fiber on the nano scale, so as to construct a precursor (gel) of a cage-shaped structure surrounded by a nano belt; in the invention, aluminum silicate fiber is taken as a main material and aluminum oxide fiber is taken as an auxiliary material, the aluminum silicate fiber and the aluminum oxide fiber are equivalent to the functions of a template agent and a propping agent, the form of gel can be formed by guiding aluminum oxide nano powder, the template effect is provided for the formation of a cage-shaped structure surrounded by nano belts, the stability and the strength of the gel structure are maintained, the follow-up normal pressure drying process is facilitated, the cage-shaped structure surrounded by the nano belts of the material is kept and enhanced stable after normal pressure drying and heat treatment, and finally, the high-temperature and high-strength aerogel material with the cage-shaped structure surrounded by the nano belts is constructed and formed, for example, as shown in fig. 2; according to the invention, if aluminum silicate fiber or aluminum oxide fiber is only added into the mixed solution containing aluminum oxide nano powder, the structure shrinkage easily occurs in the preparation process, a cage-shaped structure surrounded by the nano belt cannot be formed, the specific surface area of the formed aerogel material is obviously reduced, the density is increased, larger gaps and interfaces possibly exist, heat transfer is more scattered, the heat conductivity is obviously increased, and the heat insulation performance is reduced. According to the invention, if the alumina nano powder is subjected to hydrothermal reaction with mullite fiber, basalt fiber or glass fiber and other fibers, only physical doping and intertwining between the alumina aerogel and the fibers can be realized, and the aerogel material with a cage-shaped structure surrounded by the nano belt can not be formed.
Compared with the traditional pearl necklace aerogel material, the high-temperature-resistant high-strength aerogel material prepared by the invention is a cage-shaped nano structure surrounded by nano belts, the porosity can be more than 90 percent, the super-light aerogel material has super-light property and can be as low as 0.2g/cm 3 About, the heat-resistant temperature can reach more than 1200 ℃, the long-time heat insulation application at 1200 ℃ can be realized, and the heat-resistant material has better mechanical strength; the high-temperature-resistant high-strength aerogel material has the advantages of good temperature resistance, high strength, low density and good heat insulation performance.
The method can directly obtain the high-temperature-resistant high-strength aerogel material through normal-pressure drying and relatively low-temperature heat treatment steps after the gel is soaked in water, and the supercritical drying process and the complicated step-by-step heat treatment process or the relatively high-temperature heat treatment process can simplify the preparation process flow, reduce the process steps and the operation difficulty, reduce the complexity and the cost of the preparation process, help to save energy sources and avoid environmental pollution and waste caused by using an organic solvent. The method adopts the steps which are simpler, more environment-friendly and easier to control, and is favorable for obtaining the high-temperature-resistant high-strength aerogel material with more stable quality and more excellent performance.
According to some preferred embodiments, the mass fraction of alumina nano-powder contained in the mixed solution is 5-20% (e.g. 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14%, 15%, 16%, 17%, 18%, 19% or 20%), more preferably 8-20%.
According to some preferred embodiments, the mixture contains 1 to 15% (e.g. 1%, 2%, 3%, 4%, 5%, 6%, 7%, 8%, 9%, 10%, 11%, 12%, 13%, 14% or 15%), preferably 1 to 4% (e.g. 1%, 2%, 3% or 4%) of the sum of the mass fractions of aluminium silicate fibres and aluminium oxide fibres.
According to some preferred embodiments, the mass ratio of the aluminum silicate fiber to the aluminum oxide fiber is (1 to 3): 1 (e.g., 1:1, 1.5:1, 2:1, 2.5:1, or 3:1), preferably 2:1.
In the present invention, it is preferable that the mass ratio of the aluminum silicate fiber to the aluminum oxide fiber is (1 to 3): 1, through reasonable proportion, the advantages of the alumina silicate and the alumina silicate can be comprehensively exerted, better comprehensive performance is obtained, the high-temperature-resistant high-strength aerogel material with better performance is facilitated to be obtained, and if the proportion of the alumina silicate fiber and the alumina silicate fiber is not in a reasonable range, the pore structure and the skeleton strength of the aerogel material can be influenced, so that the porosity, the specific surface area, the heat conductivity coefficient and the like of the aerogel material are influenced.
The invention does not limit the alumina nano powder, the aluminum silicate fiber and the alumina fiber, and products which can be directly purchased in the market or synthesized by the prior method can be adopted; preferably, the particle size of the alumina nano powder is 10-100 nm, preferably 10-25 nm; the length of the aluminum silicate fiber is 1-3 mm, the diameter is 2-9 mu m, the length of the aluminum oxide fiber is 1-5 mm, and the diameter is 4-9 mu m.
According to some preferred embodiments, the time of the hydrothermal reaction is 1 to 48 hours (e.g. 1, 3, 5, 10, 12, 15, 18, 20, 25, 30, 36, 40, 45 or 48 hours), preferably 3 to 12 hours (e.g. 3, 4, 5, 6, 7, 8, 9, 10, 11 or 12 hours); and/or the soaking time is 6-72 hours (e.g., 6, 12, 18, 24, 30, 36, 42, 48, 60, 66, or 72 hours). In the present invention, the soaking is performed at room temperature, for example, at room temperature of 20 to 35 ℃ in water for 6 to 72 hours.
According to some preferred embodiments, the temperature of the atmospheric drying is 25 to 80 ℃ (e.g. 25 ℃, 30 ℃, 35 ℃, 40 ℃, 45 ℃, 50 ℃, 55 ℃, 60 ℃, 65 ℃, 70 ℃, 75 ℃ or 80 ℃), and the time of the atmospheric drying is 12 to 120 hours (e.g. 12, 24, 36, 48, 60, 72, 84, 96, 108 or 120 hours), preferably 24 to 48 hours.
According to some preferred embodiments, the temperature of the heat treatment is 600 to 1000 ℃ (e.g. 600 ℃, 700 ℃, 800 ℃, 900 ℃ or 1000 ℃), preferably 600 to 800 ℃ (e.g. 600 ℃, 700 ℃ or 800 ℃), and the time of the heat treatment is 0.5 to 2 hours (e.g. 0.5, 1, 1.5 or 2 hours).
Compared with the heat treatment at the relatively low temperature of 600-1000 ℃, the heat treatment at the relatively high temperature of 1000-1200 ℃ can prepare the high-temperature-resistant high-strength aerogel material with equivalent effect.
According to some embodiments, the concentration of the hydrochloric acid is 0.1 to 5mol/L, preferably 1 to 5mol/L; and/or the amount of the hydrochloric acid is 0.3 to 5% by weight, preferably 1 to 3% by weight of the total mass of the mixed solution.
According to some specific embodiments, the preparation process of the high temperature resistant high strength aerogel material according to the present invention is shown in fig. 1, for example, and the preparation method includes the following steps:
(1) Uniformly mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid (hydrochloric acid solution) by using water to obtain a mixed solution, uniformly mixing the alumina nano powder, the aluminum silicate fiber and the alumina fiber by using a high-speed dispersing machine, and then placing the mixed solution into a hydrothermal reaction at 150-300 ℃ for 1-48 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 5-20%, and the sum of the mass fractions of the aluminum silicate fiber and the alumina fiber contained in the mixed solution is 1-15%; in step (1), for example, the components are uniformly mixed by a high-speed dispersion method, specifically: mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, and then dispersing at a high speed for 5-120min in a high-speed dispersing machine at a rotating speed of 1000-8000 r/min; in the invention, the mixed solution is put into a closed container for hydrothermal reaction at 150-300 ℃; in the invention, the hydrothermal reaction needs to be carried out under a closed condition, and the material of the closed container needs to be a material which does not react with the system;
(2) Soaking the obtained gel in pure water for 6-72h;
(3) Performing normal pressure drying on the obtained soaking gel material, wherein the normal pressure drying temperature is 25-80 ℃, and the normal pressure drying time is 12-120 hours, so as to obtain an aerogel material; the atmospheric drying is, for example, oven drying under atmospheric pressure;
(4) And carrying out heat treatment on the dried aerogel material, wherein the heat treatment temperature is 600-1000 ℃.
According to some preferred embodiments, the high-temperature-resistant high-strength aerogel material has a cage structure surrounded by nano belts, for example, as shown in fig. 2, fig. 2 shows that the high-temperature-resistant high-strength aerogel material prepared by the method has a cage structure surrounded by nano belts, and specifically, the skeleton structure of the high-temperature-resistant high-strength aerogel material in the method is a cage structure surrounded by nano belts.
According to some preferred embodiments, the density of the high temperature resistant high strength aerogel material is as low as 0.2g/cm 3 The porosity is high as 93.5%, and the specific surface area is not less than 152m 2 The compression strength at 10% compression per gram is as high as 1.3MPa, the heat conductivity coefficient is as low as 0.040W/(m.K), and the heat-resistant temperature is above 1200 ℃.
The present invention provides in a second aspect, high temperature resistant, high strength aerogel materials made by the method of the present invention described in the first aspect.
The invention will be further illustrated by way of example, but the scope of the invention is not limited to these examples.
Example 1
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 2%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
(2) And (3) placing the obtained gel in pure water, and soaking for 24 hours at the room temperature of 25 ℃ to obtain the soaked gel.
(3) And (3) performing normal-pressure drying on the obtained soaking treatment gel, wherein the normal-pressure drying temperature is 60 ℃, and the normal-pressure drying time is 24 hours, so as to obtain the aerogel material.
(4) Performing heat treatment on the obtained aerogel material to obtain a high-temperature-resistant high-strength aerogel material; the heat treatment temperature is 600 ℃, the heat treatment time is 1h, and the heat treatment is carried out under the air atmosphere.
The high-temperature-resistant high-strength aerogel material prepared by the embodiment has good structural strength, and when the heat insulation performance test is carried out, the surface of the high-temperature-resistant high-strength aerogel material is found to be free from light loss, color change and falling.
The density of the high-temperature resistant high-strength aerogel material prepared in the embodiment is 0.2g/cm 3 The thermal conductivity (coefficient of thermal conductivity) at room temperature was 0.040W/(mK), the specific surface area was 152m 2 The high-temperature resistant high-strength aerogel material has the advantages of high temperature resistance, large specific surface area, small porosity, high strength, low density and good heat insulation performance, wherein the porosity is 93.5%, the compression strength is 1.3MPa under the compression of 10%, and the heat resistance temperature is 1200 ℃; wherein, the test of heat-resistant temperature is: the aerogel materials finally prepared in each example were heat treated (air atmosphere) at a certain high temperature for 2 hours, the linear shrinkage of the aerogel materials was not more than 5%, indicating that the aerogel materials were able to withstand the high temperature; for the embodiment, the high-temperature-resistant high-strength aerogel material prepared by the embodiment is subjected to heat treatment (air atmosphere) for 2 hours at 1200 ℃, the linear shrinkage rate of the aerogel material is not more than 5%, the heat-resistant temperature is 1200 ℃, and the long-time heat insulation application at 1200 ℃ can be realized.
Example 2
Example 2 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, alumina fiber and hydrochloric acid with water, dispersing for 30min in a high-speed dispersing machine at a rotation speed of 5000r/min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10 percent, and the mass fraction of the alumina fiber contained in the mixed solution is 3 percent; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The aerogel materials prepared in the steps (1) to (4) in this example have good structural strength, but shrink greatly in the normal pressure drying process, the density of the material is large, the specific surface area is small, the thermal conductivity coefficient is obviously increased, and the performance test results are shown in table 1.
Example 3
Example 3 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber and hydrochloric acid by using water, dispersing for 30min in a high-speed dispersing machine at a rotation speed of 5000r/min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10 percent, and the mass fraction of the aluminum silicate fiber contained in the mixed solution is 3 percent; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The aerogel materials prepared in steps (1) to (4) of this example have good structural strength, but shrink in the normal pressure drying process, the density of the material is large, the specific surface area is small, the thermal conductivity is increased, and the performance test results are shown in table 1.
Example 4
Example 4 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 0.5%, and the mass fraction of the alumina fiber contained in the mixed solution is 0.5%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The performance test results of the high temperature resistant high strength aerogel materials prepared in steps (1) to (4) of this example are shown in table 1.
Example 5
Example 5 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 10%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) in this example are shown in table 1.
Example 6
Example 6 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution in a hydrothermal reaction at 150 ℃ for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 2%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
In this example, the hydrothermal reaction temperature was low, a very complete block could not be formed, shrinkage of the aerogel material occurred, and the porosity and specific surface area of the produced aerogel material were significantly reduced, and other performance test results are shown in table 1.
Example 7
Example 7 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 25%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 2%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) in this example are shown in table 1.
The aerogel materials prepared in the steps (1) to (4) of the embodiment have very good structural strength, but the specific surface area of the material is very small, and the heat conductivity coefficient is obviously increased.
Example 8
Example 8 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 4%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 2%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) in this example are shown in table 1.
Example 9
Example 9 is substantially the same as example 1 except that:
(4) Performing heat treatment on the obtained aerogel material to obtain a high-temperature-resistant high-strength aerogel material; the heat treatment temperature is 500 ℃, the heat treatment time is 1h, and the heat treatment is carried out under the air atmosphere.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) in this example are shown in table 1.
Comparative example 1
Comparative example 1 is substantially the same as example 1 except that:
(2) Aging the obtained gel for 2 hours in an unsealed environment in air at 60 ℃ to obtain an aged gel block; and (3) adopting the aged gel block to carry out the subsequent step (3) and the step (4).
The results of the performance test of the aerogel materials prepared in steps (1) to (4) of this comparative example are shown in table 1.
Comparative example 2
Comparative example 2 is substantially the same as example 1 except that:
(1) Mixing alumina nano powder, mullite fiber, basalt fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at a rotation speed of 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the mullite fiber contained in the mixed solution is 2%, and the mass fraction of the basalt fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) of this comparative example are shown in table 1.
Comparative example 3
(1) Mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water, dispersing in a high-speed dispersing machine at 5000r/min for 30min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the mass fraction of the aluminum silicate fiber contained in the mixed solution is 2%, and the mass fraction of the alumina fiber contained in the mixed solution is 1%; the dosage of the hydrochloric acid is 1.5 percent of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
(2) Aging the gel for 2 hours in a non-sealing environment in air at 60 ℃ to obtain the aged gel.
(3) Sequentially performing solvent replacement and supercritical drying on the aged gel to obtain an aerogel material; the method comprises the following specific steps: the solvent replacement adopts ethanol as a solvent, and after 3 times of replacement is carried out according to 10 times of the volume of the gel block after the soaking treatment, the time of each solvent replacement is 3 days; then, a supercritical carbon dioxide drying process is carried out, wherein the temperature of supercritical drying is 50 ℃, the pressure is 14MPa, and the time is 24 hours.
(4) Performing heat treatment on the obtained aerogel to obtain a composite aerogel material; the heat treatment temperature is 1150 ℃, the heat treatment time is 0.5h, and the heat treatment is carried out under the air atmosphere.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) of this comparative example are shown in table 1.
Comparative example 4
Comparative example 4 is substantially the same as example 1 except that:
(1) Mixing the alumina nano powder with hydrochloric acid by using water, dispersing for 30min in a high-speed dispersing machine at a rotation speed of 5000r/min, and uniformly mixing to obtain a mixed solution; then placing the mixed solution into 220 ℃ for hydrothermal reaction for 5 hours to obtain gel; the mass fraction of the alumina nano powder contained in the mixed solution is 10%, the using amount of the hydrochloric acid is 1.5% of the total weight of the mixed solution, and the concentration of the hydrochloric acid is 2mol/L.
The results of the performance test of the aerogel materials prepared in steps (1) to (4) of this comparative example are shown in table 1.
In table 1, the symbol "-" indicates that the performance index was not tested.
The invention is not described in detail in a manner known to those skilled in the art.
Finally, it should be noted that: the above embodiments are only for illustrating the technical solution of the present invention, and are not limiting; although the invention has been described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that: the technical scheme described in the foregoing embodiments can be modified or some technical features thereof can be replaced by equivalents; such modifications and substitutions do not depart from the spirit and scope of the technical solutions of the embodiments of the present invention.
Claims (10)
1. The preparation method of the high-temperature-resistant high-strength aerogel material is characterized by comprising the following steps of:
(1) Uniformly mixing alumina nano powder, aluminum silicate fiber, alumina fiber and hydrochloric acid with water to obtain a mixed solution, and then placing the mixed solution at 150-300 ℃ for hydrothermal reaction to obtain gel;
(2) Soaking the gel in water to obtain a soaked gel;
(3) Drying the soaking treatment gel obtained in the step (2) at normal pressure to obtain an aerogel material;
(4) And (3) performing heat treatment on the aerogel material obtained in the step (3) to obtain the high-temperature-resistant high-strength aerogel material.
2. The method of manufacturing according to claim 1, characterized in that:
the mass fraction of the alumina nano powder contained in the mixed solution is 5-20%.
3. The method of manufacturing according to claim 1, characterized in that:
the mixed solution contains 1-15% of the sum of the mass fractions of aluminum silicate fiber and aluminum oxide fiber.
4. The method of manufacturing according to claim 1, characterized in that:
the mass ratio of the aluminum silicate fiber to the aluminum oxide fiber is (1-3): 1, preferably 2:1.
5. The method of manufacturing according to claim 1, characterized in that:
the hydrothermal reaction time is 1-48 h, preferably 3-12 h; and/or
The soaking time is 6-72 h.
6. The method of manufacturing according to claim 1, characterized in that:
the temperature of the normal pressure drying is 25-80 ℃, and the time of the normal pressure drying is 12-120 h.
7. The method of manufacturing according to claim 1, characterized in that:
the temperature of the heat treatment is 600-1000 ℃, and the time of the heat treatment is 0.5-2 h.
8. The method of manufacturing according to claim 1, characterized in that:
the concentration of the hydrochloric acid is 0.1-5 mol/L; and/or
The dosage of the hydrochloric acid accounts for 0.3-5% of the total mass of the mixed solution.
9. The production method according to any one of claims 1 to 8, characterized in that:
the high-temperature-resistant high-strength aerogel material has a cage-like structure surrounded by a nano belt.
10. A high temperature and high strength aerogel material produced by the production process of any one of claims 1 to 9.
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