CN115432977B - Preparation method of silica aerogel fiber composite material - Google Patents
Preparation method of silica aerogel fiber composite material Download PDFInfo
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- CN115432977B CN115432977B CN202211324155.1A CN202211324155A CN115432977B CN 115432977 B CN115432977 B CN 115432977B CN 202211324155 A CN202211324155 A CN 202211324155A CN 115432977 B CN115432977 B CN 115432977B
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- 239000000835 fiber Substances 0.000 title claims abstract description 54
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 31
- 239000002131 composite material Substances 0.000 title claims abstract description 31
- 239000004965 Silica aerogel Substances 0.000 title claims abstract description 29
- 238000002360 preparation method Methods 0.000 title claims abstract description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 37
- 239000004964 aerogel Substances 0.000 claims abstract description 33
- 238000001035 drying Methods 0.000 claims abstract description 23
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 238000003756 stirring Methods 0.000 claims abstract description 19
- 238000000034 method Methods 0.000 claims abstract description 18
- 239000000843 powder Substances 0.000 claims abstract description 17
- 239000002002 slurry Substances 0.000 claims abstract description 15
- 238000001291 vacuum drying Methods 0.000 claims abstract description 15
- 238000007710 freezing Methods 0.000 claims abstract description 14
- 230000008014 freezing Effects 0.000 claims abstract description 14
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002270 dispersing agent Substances 0.000 claims abstract description 13
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 13
- 239000010703 silicon Substances 0.000 claims abstract description 13
- 239000004094 surface-active agent Substances 0.000 claims abstract description 13
- 238000002156 mixing Methods 0.000 claims abstract description 11
- 239000003607 modifier Substances 0.000 claims abstract description 11
- 239000002994 raw material Substances 0.000 claims abstract description 11
- 239000011230 binding agent Substances 0.000 claims abstract description 10
- 238000000227 grinding Methods 0.000 claims abstract description 8
- 239000003054 catalyst Substances 0.000 claims abstract description 7
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 26
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical compound CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 24
- 238000002791 soaking Methods 0.000 claims description 21
- 239000000243 solution Substances 0.000 claims description 21
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 14
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical group CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 claims description 14
- IJOOHPMOJXWVHK-UHFFFAOYSA-N chlorotrimethylsilane Chemical group C[Si](C)(C)Cl IJOOHPMOJXWVHK-UHFFFAOYSA-N 0.000 claims description 14
- 238000006243 chemical reaction Methods 0.000 claims description 13
- 238000004321 preservation Methods 0.000 claims description 10
- 239000004568 cement Substances 0.000 claims description 9
- 239000004354 Hydroxyethyl cellulose Substances 0.000 claims description 7
- 229920000663 Hydroxyethyl cellulose Polymers 0.000 claims description 7
- 229910021529 ammonia Inorganic materials 0.000 claims description 7
- IXCSERBJSXMMFS-UHFFFAOYSA-N hcl hcl Chemical compound Cl.Cl IXCSERBJSXMMFS-UHFFFAOYSA-N 0.000 claims description 7
- 235000019447 hydroxyethyl cellulose Nutrition 0.000 claims description 7
- 239000011259 mixed solution Substances 0.000 claims description 7
- 239000005051 trimethylchlorosilane Substances 0.000 claims description 7
- 239000003377 acid catalyst Substances 0.000 claims description 6
- 239000011490 mineral wool Substances 0.000 claims description 5
- 239000000919 ceramic Substances 0.000 claims description 4
- 239000003513 alkali Substances 0.000 claims description 3
- 239000003365 glass fiber Substances 0.000 claims description 3
- 239000002184 metal Substances 0.000 claims description 3
- 239000012209 synthetic fiber Substances 0.000 claims description 3
- 229920002994 synthetic fiber Polymers 0.000 claims description 3
- 239000002585 base Substances 0.000 claims description 2
- 238000006073 displacement reaction Methods 0.000 claims description 2
- 230000004048 modification Effects 0.000 claims description 2
- 238000012986 modification Methods 0.000 claims description 2
- 239000000853 adhesive Substances 0.000 claims 1
- 230000001070 adhesive effect Effects 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 3
- 238000009413 insulation Methods 0.000 abstract description 2
- 235000012239 silicon dioxide Nutrition 0.000 abstract description 2
- 230000032683 aging Effects 0.000 abstract 1
- 230000003301 hydrolyzing effect Effects 0.000 abstract 1
- 239000000377 silicon dioxide Substances 0.000 abstract 1
- 235000019441 ethanol Nutrition 0.000 description 17
- 230000000052 comparative effect Effects 0.000 description 6
- 150000001298 alcohols Chemical class 0.000 description 5
- 238000001000 micrograph Methods 0.000 description 3
- 230000007547 defect Effects 0.000 description 2
- 238000000352 supercritical drying Methods 0.000 description 2
- 229920000742 Cotton Polymers 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000002612 dispersion medium Substances 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 238000004108 freeze drying Methods 0.000 description 1
- 229910052500 inorganic mineral Inorganic materials 0.000 description 1
- 239000011707 mineral Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000000465 moulding Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000007783 nanoporous material Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 235000011837 pasties Nutrition 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 239000000779 smoke Substances 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000011343 solid material Substances 0.000 description 1
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- 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
- 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
- C04B28/02—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 hydraulic cements other than calcium sulfates
- C04B28/04—Portland cements
-
- 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
- C04B14/00—Use of inorganic materials as fillers, e.g. pigments, for mortars, concrete or artificial stone; Treatment of inorganic materials specially adapted to enhance their filling properties in mortars, concrete or artificial stone
- C04B14/02—Granular materials, e.g. microballoons
- C04B14/04—Silica-rich materials; Silicates
- C04B14/06—Quartz; Sand
- C04B14/064—Silica aerogel
-
- 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
- C04B2201/20—Mortars, concrete or artificial stone characterised by specific physical values for the density
-
- 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)
- Dispersion Chemistry (AREA)
- Civil Engineering (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Inorganic Chemistry (AREA)
- Silicon Compounds (AREA)
Abstract
A preparation method of a silicon dioxide aerogel fiber composite material comprises the steps of mixing a silicon source, a dispersing agent, a catalyst and deionized water, and fully hydrolyzing and polycondensing raw materials; transferring the obtained sol into a container, and putting the container into a water bath kettle for constant-temperature water bath gel aging; replacing the gel obtained by using a replacement agent at room temperature, modifying the gel by using a modifier once, and replacing the gel by using the replacement agent once; transferring the obtained material into a vacuum drying oven, and gradient drying at different temperatures; grinding the obtained pure aerogel into fine powder, mixing with a binder, a surfactant and fibers in deionized water, and fully stirring; transferring the slurry into a mould, putting the mould into a freeze dryer, freezing at low temperature, and vacuumizing and drying to obtain the silica aerogel fiber composite material. The method has low cost and strong process adaptability, the prepared silica aerogel fiber composite material has good formability and good heat insulation performance, and the directional doping of fibers can be realized.
Description
Technical Field
The invention relates to a preparation method of a nano porous material, in particular to a preparation method of a silica aerogel fiber composite material.
Background
Aerogel is a highly dispersed solid material, also called "solid smoke", in which nano-scale colloidal particles are aggregated with each other to form a nano-porous network structure, and the pores are filled with a gaseous dispersion medium. Owing to the nano porous structure, the aerogel has excellent physical properties of high porosity, high specific surface area, low thermal conductivity, low density and the like, is a novel nano material with excellent performance, and is widely applied to the fields of building heat preservation, aerospace, energy storage, conversion and the like. In practical application, a fiber composite method is often adopted to improve the mechanical properties of the silica aerogel so as to meet the practical engineering requirements.
The existing aerogel material preparation methods are mostly based on a sol-gel method, and the common aerogel preparation methods can be divided into three types according to different drying modes: 1) The normal pressure drying method has the lowest cost, but the product performance is relatively poor; 2) The freeze drying method has moderate cost, but is mostly limited to the preparation of organic aerogel; 3) The supercritical drying method has the advantages of optimal product performance, highest cost and complex equipment requirement. Based on the characteristics of the above methods, there is a need to develop a novel preparation method of silica aerogel composite materials, which can be widely used.
Disclosure of Invention
The invention aims to provide a preparation method of a silica aerogel fiber composite material with low cost and good formability.
In order to achieve the above purpose, the invention adopts the following technical scheme:
1) 1 part of silicon source, 5 parts of deionized water and 2.5 parts of dispersing agent are respectively taken according to mole parts and evenly mixed, and then 2.4X10 are added -3 Fully mixing and stirring acid catalyst to make silicon source fully hydrolyze in solution, then adding 3.6X10 -3 Stirring the alkali catalyst to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath, adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction to form uniform and stable alcohol gel;
3) Soaking and replacing the alcogel with a replacement agent at room temperature, soaking and modifying the alcogel with a modifier for one time, and soaking and replacing the alcogel with the replacement agent for one time to obtain a modified alcogel;
4) Transferring the modified alcogel into a vacuum drying oven, carrying out gradient drying at different temperatures to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) 1-20 parts of pure aerogel fine powder, 100 parts of deionized water, 1-2 parts of binder, 2 parts of surfactant and 0.2-5 parts of fiber are taken according to parts by mass, mixed and fully stirred to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer, freezing at low temperature, and vacuumizing and drying to obtain the silica aerogel fiber composite material.
The silicon source is tetraethyl orthosilicate (TEOS), and the dispersing agent is freeAqueous ethanol, 0.1mol/L hydrochloric acid (HCl) solution as acid catalyst, 1mol/L ammonia (NH) 3 ·H 2 O) solution.
And stirring for 1h after adding the acid catalyst, and stirring for 5-15min after adding the base catalyst.
The temperature of the constant-temperature water bath in the step 2) is 50 ℃, and the heat preservation time is 3 days.
The displacer in the step 3) is n-hexane, the time of each displacement is 48 hours, the modifier is trimethylchlorosilane, and the time of each modification is 24 hours.
The different temperature gradients in the step 4) are 40 ℃, 60 ℃, 80 ℃ and 100 ℃, and the drying time period of each temperature stage is 2 hours.
The binder in the step 5) is white cement, the surfactant is hydroxyethyl cellulose, and the fiber is one or more of plant fiber, synthetic fiber, glass fiber, mineral wool fiber, ceramic fiber and metal fiber.
The low-temperature freezing temperature of the step 6) is minus 75 ℃, the freezing time is 24 hours, the vacuum drying pressure is less than 5Pa, and the drying time is 2-3 days.
Aiming at the defects of the aerogel preparation method in the background art, the invention designs a preparation method of the silica aerogel fiber composite material with low cost and good formability by taking a silicon source, deionized water, a catalyst, a dispersing agent, a modifier, fibers, a binder and a surfactant as raw materials. The method avoids the higher equipment requirement of the supercritical drying method, greatly improves the molding performance of the product while ensuring lower cost, can realize complex shape effect, has customizable product shape, simultaneously retains the most important low thermal conductivity performance of the aerogel composite material, and has the potential of large-scale popularization and application.
The invention has the advantages that:
the method has the advantages of simple raw material and equipment requirements, low cost, easy large-scale application and strong process adaptability, can use different common fibers as raw materials, overcomes the defect of the formability of the pure silica aerogel by a simple and rapid fiber compounding method, can customize complex shapes according to requirements, can realize directional doping of the fibers, and expands the application range of preparing the aerogel by a normal pressure drying method.
Drawings
FIG. 1 is an external view of a silica aerogel composite prepared in example 1;
FIG. 2 is a scanning electron microscope image of the silica aerogel composite prepared in example 1;
FIG. 3 is a cross-sectional fiber orientation diagram of a silica aerogel composite prepared in accordance with the comparative example.
FIG. 4 is a scanning electron microscope image of a silica aerogel composite prepared in accordance with the comparative example.
Detailed Description
Example 1:
1) 1 part of Tetraethoxysilane (TEOS) and 5 parts of deionized water are respectively taken according to the mol parts and evenly mixed with 2.5 parts of absolute ethyl alcohol, and then 2.4X10 are added -3 The silicon source is fully hydrolyzed in the solution by fully mixing and stirring 0.1mol/L hydrochloric acid (HCl) solution for 1h, and then 3.6X10 g is added -3 1mol/L ammonia (NH) 3 ·H 2 Stirring the solution for 5min to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath at 50 ℃, simultaneously adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction for 3 days to enable a reaction system to form uniform and stable alcogel;
3) Soaking and replacing the alcohol gel with a displacer n-hexane for 48 hours at room temperature, then soaking and modifying the alcohol gel with a modifier trimethylchlorosilane for 24 hours, and then soaking and replacing the alcohol gel with the displacer n-hexane for 48 hours to obtain a modified alcohol gel;
4) Transferring the modified alcogel into a vacuum drying oven, respectively drying at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ for 2 hours to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) 10 parts of pure aerogel fine powder, 100 parts of deionized water, 1 part of binder white cement, 2 parts of surfactant hydroxyethyl cellulose and 0.5 part of rock wool fiber are taken according to parts by mass and mixed, and fully stirred to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer at the temperature of minus 90 ℃, freezing for 24 hours at low temperature, and then vacuumizing and drying for 3 days at the vacuum drying pressure of 1Pa to obtain the silica aerogel fiber composite material.
It can be seen from fig. 1 that the material obtained by the preparation process exhibits excellent formability, and that samples with complicated lines and shapes can be obtained, with excellent shape customization potential.
From fig. 2, it can be seen that the fibers form a well-blended structure with the aerogel powder, which encapsulates the fibers, which form the skeletal support.
Example 2:
1) 1 part of Tetraethoxysilane (TEOS) and 5 parts of deionized water are respectively taken according to the mol parts and evenly mixed with 2.5 parts of absolute ethyl alcohol, and then 2.4X10 are added -3 The silicon source is fully hydrolyzed in the solution by fully mixing and stirring 0.1mol/L hydrochloric acid (HCl) solution for 1h, and then 3.6X10 g is added -3 1mol/L ammonia (NH) 3 ·H 2 Stirring the solution for 10min to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath at 50 ℃, simultaneously adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction for 3 days to enable a reaction system to form uniform and stable alcogel;
3) Soaking and replacing the alcohol gel with a displacer n-hexane for 48 hours at room temperature, then soaking and modifying the alcohol gel with a modifier trimethylchlorosilane for 24 hours, and then soaking and replacing the alcohol gel with the displacer n-hexane for 48 hours to obtain a modified alcohol gel;
4) Transferring the modified alcogel into a vacuum drying oven, respectively drying at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ for 2 hours to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) 15 parts of pure aerogel fine powder, 100 parts of deionized water, 2 parts of binder white cement, 2 parts of surfactant hydroxyethyl cellulose and 0.5 part of glass fiber are taken according to parts by mass and mixed, and fully stirred to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer at the temperature of minus 90 ℃, freezing for 24 hours at low temperature, and then vacuumizing and drying for 3 days at the vacuum drying pressure of 1Pa to obtain the silica aerogel fiber composite material.
Comparative example
100g of deionized water, 2g of white cement, 2g of surfactant and 1g of rock wool fiber are taken, the white cement and the surfactant are added into the deionized water, mixed and stirred to be in a viscous state, a small amount of silica aerogel powder is added for multiple times, and fully stirred, finally the rock wool fiber is added, fully stirred, the obtained pasty mixture is transferred into a special directional freezing mold, and is put into a freeze dryer, frozen for 24 hours at the low temperature of minus 90 ℃, and then dried for 3 days in the environment of 1Pa, so that the final directional fiber aerogel composite material is obtained.
Table 1 density and thermal conductivity of examples
| Sample of | Density of | Thermal conductivity |
| Example 1 | 0.076 | 0.0302 |
| Example 2 | 0.095 | 0.0306 |
| Comparative example | 0.039 | 0.0349 |
From fig. 3 and 4, it can be seen that the macroscopic section and microscopic electron microscope images of the sample prepared by the special directional freezing mold show obvious directional arrangement structure, which indicates that the composite material obtained by the method can realize the directional doping of the fiber.
It can be seen from table 1 that the samples obtained by the preparation method have lower thermal conductivity, exhibit better heat insulation performance, and the thermal conductivity of the comparative examples is higher than that of examples 1 and 2, mainly because the fibers of the comparative examples have better orientation, and the thermal conductivity along the fiber arrangement direction is improved.
Example 3:
1) 1 part of Tetraethoxysilane (TEOS) and 5 parts of deionized water are respectively taken according to the mol parts and evenly mixed with 2.5 parts of absolute ethyl alcohol, and then 2.4X10 are added -3 The silicon source is fully hydrolyzed in the solution by fully mixing and stirring 0.1mol/L hydrochloric acid (HCl) solution for 1h, and then 3.6X10 g is added -3 1mol/L ammonia (NH) 3 ·H 2 Stirring the solution for 15min to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath at 50 ℃, simultaneously adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction for 3 days to enable a reaction system to form uniform and stable alcogel;
3) Soaking and replacing the alcohol gel with a displacer n-hexane for 48 hours at room temperature, then soaking and modifying the alcohol gel with a modifier trimethylchlorosilane for 24 hours, and then soaking and replacing the alcohol gel with the displacer n-hexane for 48 hours to obtain a modified alcohol gel;
4) Transferring the modified alcogel into a vacuum drying oven, respectively drying at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ for 2 hours to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) Mixing 20 parts of pure aerogel fine powder, 100 parts of deionized water, 1.8 parts of binder white cement, 2 parts of surfactant hydroxyethyl cellulose, 5 parts of synthetic fibers and mineral cotton fibers with ceramic fibers according to parts by mass, and fully stirring to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer at the temperature of minus 80 ℃, freezing for 24 hours at low temperature, and then vacuumizing and drying for 2 days at the vacuum drying pressure of 2Pa to obtain the silica aerogel fiber composite material.
Example 4:
1) Pressing the buttonMixing 1 part tetraethyl orthosilicate (TEOS), 5 parts deionized water and 2.5 parts absolute ethyl alcohol uniformly, and adding 2.4X10 g -3 The silicon source is fully hydrolyzed in the solution by fully mixing and stirring 0.1mol/L hydrochloric acid (HCl) solution for 1h, and then 3.6X10 g is added -3 1mol/L ammonia (NH) 3 ·H 2 Stirring the solution for 8min to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath at 50 ℃, simultaneously adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction for 3 days to enable a reaction system to form uniform and stable alcogel;
3) Soaking and replacing the alcohol gel with a displacer n-hexane for 48 hours at room temperature, then soaking and modifying the alcohol gel with a modifier trimethylchlorosilane for 24 hours, and then soaking and replacing the alcohol gel with the displacer n-hexane for 48 hours to obtain a modified alcohol gel;
4) Transferring the modified alcogel into a vacuum drying oven, respectively drying at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ for 2 hours to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) 1 part of pure aerogel fine powder, 100 parts of deionized water, 1.2 parts of binder white cement, 2 parts of surfactant hydroxyethyl cellulose and 0.2 part of metal fiber are taken according to parts by mass and mixed, and fully stirred to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer at the temperature of minus 95 ℃, freezing for 24 hours at low temperature, and then vacuumizing and drying for 2 days at the vacuum drying pressure of 4Pa to obtain the silica aerogel fiber composite material.
Example 5:
1) 1 part of Tetraethoxysilane (TEOS) and 5 parts of deionized water are respectively taken according to the mol parts and evenly mixed with 2.5 parts of absolute ethyl alcohol, and then 2.4X10 are added -3 The silicon source is fully hydrolyzed in the solution by fully mixing and stirring 0.1mol/L hydrochloric acid (HCl) solution for 1h, and then 3.6X10 g is added -3 1mol/L ammonia (NH) 3 ·H 2 Stirring the solution for 12min to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath at 50 ℃, simultaneously adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction for 3 days to enable a reaction system to form uniform and stable alcogel;
3) Soaking and replacing the alcohol gel with a displacer n-hexane for 48 hours at room temperature, then soaking and modifying the alcohol gel with a modifier trimethylchlorosilane for 24 hours, and then soaking and replacing the alcohol gel with the displacer n-hexane for 48 hours to obtain a modified alcohol gel;
4) Transferring the modified alcogel into a vacuum drying oven, respectively drying at 40 ℃, 60 ℃, 80 ℃ and 100 ℃ for 2 hours to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) Mixing 5 parts of pure aerogel fine powder, 100 parts of deionized water, 1.5 parts of binder white cement, 2 parts of surfactant hydroxyethyl cellulose and 3 parts of ceramic fibers according to parts by mass, and fully stirring to obtain slurry;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer at the temperature of minus 100 ℃, freezing for 24 hours at low temperature, and then vacuumizing and drying for 3 days at the vacuum drying pressure of 3Pa to obtain the silica aerogel fiber composite material.
Claims (7)
1. The preparation method of the silica aerogel fiber composite material is characterized by comprising the following steps:
1) 1 part of silicon source, 5 parts of deionized water and 2.5 parts of dispersing agent are respectively taken according to mole parts and evenly mixed, and then 2.4X10 are added -3 Fully mixing and stirring acid catalyst to make silicon source fully hydrolyze in solution, then adding 3.6X10 -3 Stirring the alkali catalyst to fully hydrolyze and polycondense the raw materials to obtain a mixed solution;
2) Transferring the mixed sol into a container, putting the container into a water bath kettle, carrying out constant-temperature water bath, adding 2.5 parts of dispersing agent, and carrying out heat preservation reaction to form uniform and stable alcohol gel;
3) Soaking and replacing the alcogel with a replacement agent at room temperature, soaking and modifying the alcogel with a modifier for one time, and soaking and replacing the alcogel with the replacement agent for one time to obtain a modified alcogel;
4) Transferring the modified alcogel into a vacuum drying oven, carrying out gradient drying at different temperatures to obtain pure aerogel, and grinding the pure aerogel into fine powder;
5) 1-20 parts of pure aerogel fine powder, 100 parts of deionized water, 1-2 parts of binder, 2 parts of surfactant and 0.2-5 parts of fiber are taken according to parts by mass, mixed and fully stirred to obtain slurry;
the adhesive is white cement, and the surfactant is hydroxyethyl cellulose;
6) Transferring the slurry into a mould, putting the mould into a freeze dryer, freezing at low temperature, and vacuumizing and drying to obtain a silica aerogel fiber composite material;
the low-temperature freezing temperature is minus 75 ℃, the freezing time is 24 hours, the vacuum drying pressure is less than 5Pa, and the drying time is 2-3 days.
2. The method for preparing silica aerogel fiber composite material according to claim 1, wherein the silicon source is tetraethyl orthosilicate (TEOS), the dispersant is absolute ethanol, the acid catalyst is 0.1mol/L hydrochloric acid (HCl) solution, and the base catalyst is 1mol/L ammonia (NH 3 ·H 2 O) solution.
3. The method for preparing a silica aerogel fiber composite according to claim 1, wherein the acid catalyst is added and then stirred for 1 hour, and the alkali catalyst is added and then stirred for 5 to 15 minutes.
4. The method for preparing silica aerogel fiber composite material according to claim 1, wherein the constant temperature water bath temperature in the step 2) is 50 ℃, and the heat preservation time is 3 days.
5. The method for preparing silica aerogel fiber composite material according to claim 1, wherein the displacer in the step 3) is n-hexane, the time for each displacement is 48 hours, the modifier is trimethylchlorosilane, and the time for each modification is 24 hours.
6. The method of preparing silica aerogel fiber composite of claim 1, wherein the different temperature gradients in step 4) are 40 ℃, 60 ℃, 80 ℃, 100 ℃, and the drying time period in each temperature stage is 2h.
7. The method of preparing silica aerogel fiber composite of claim 1, wherein the fibers of step 5) are one or more of plant fibers, synthetic fibers, glass fibers, mineral wool fibers, ceramic fibers, metal fibers.
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