CN111454041A - Preparation method of fiber-reinforced silica aerogel - Google Patents
Preparation method of fiber-reinforced silica aerogel Download PDFInfo
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- CN111454041A CN111454041A CN202010280291.XA CN202010280291A CN111454041A CN 111454041 A CN111454041 A CN 111454041A CN 202010280291 A CN202010280291 A CN 202010280291A CN 111454041 A CN111454041 A CN 111454041A
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Abstract
The invention provides a preparation method of fiber-reinforced silica aerogel, which takes tetraethoxysilane and alkoxy silane as mixed precursors, deionized water as a reactant, absolute ethyl alcohol as a cosolvent, and 0.1 mol-L‑1HCl and 0.5 mol. L-1 NH3·H2O is acid-base catalyst, 0.8 percent of fiber with the length of 1mm is added for SiO2The aerogel structure is reinforced, and the sol-gel-normal pressure drying method is adopted to prepare the fiber reinforced SiO2An aerogel. The fiber-reinforced silica aerogel prepared by the preparation method disclosed by the invention is strong in hydrophobicity, stable in structure and excellent in mechanical strength and toughness.
Description
Technical Field
The invention relates to a preparation method of fiber-reinforced silica aerogel.
Background
The method comprises the steps of firstly, drawing a fiber bonding crack from the fiber bonding crack along the fiber bonding crack extension direction, wherein the fiber bonding crack is formed by drawing a fiber bonding crack from the fiber bonding crack along the fiber bonding crack extension direction, and the fiber bonding crack extension direction is changed by drawing a fiber bonding crack from the fiber bonding crack along the fiber bonding crack extension direction, wherein the fiber bonding crack extension direction is changed by drawing a fiber bonding crack energy absorption mechanism, and the fiber bonding crack extension mechanism, namely, the fiber bonding crack extension mechanism, the fiber bonding process and the fiber bonding crack extension mechanism, the fiber bonding process, and the fiber bonding process.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of fiber-reinforced silica aerogel, and the prepared silica aerogel has a stable structure and excellent mechanical strength and toughness.
The invention provides a preparation method of fiber reinforced silica aerogel, which comprises the following steps:
s1 pretreatment of fibers
S1.1, cutting short and removing slag
Cutting the fiber with a crusher to obtain chopped fiber with average length of 0.09-1.1mm, soaking in water for several times, and soaking in HCl solution for 1.5-2.5 hr.
S1.2, chemical modification
And soaking the chopped fibers in 1.0 mass percent of silane coupling agent aqueous solution for treatment for 5-6h, and fishing out and drying for later use.
S2 fiber-reinforced SiO by mixed precursor method2Aerogel preparation
S2.1, preparation of Sol
Adding tetraethoxysilane, alkoxy silane, absolute ethyl alcohol and deionized water into a beaker, uniformly stirring, adding HCl solution, adjusting the pH value to be between 3 and 4, and continuously stirring for 4 to 6 hours at the temperature of between 25 and 30 ℃ to perform full acid hydrolysis to obtain the silicon dioxide sol.
S2.1, preparation of fiber-reinforced gel
Adding the chopped fibers pretreated in the step S1,rapidly stirring and dispersing; slowly dropping NH3·H2And continuously stirring the solution O uniformly, pouring the solution O into a mold, sealing and standing to form the alcogel.
S2.3, aging treatment
Soaking the alcohol gel in a mixed solution of tetraethoxysilane and absolute ethyl alcohol, and aging for 48 hours; subsequently, the solvent replacement was carried out, and the alcogel was rinsed in n-hexane for 12h, during which the n-hexane was replaced every 6 h.
S2.4, drying by stages under normal pressure
The aged fiber gel is subjected to normal pressure grading drying method to prepare hydrophobic fiber reinforced SiO2An aerogel composite.
Further, tetraethoxysilane, alkoxy silane, absolute ethyl alcohol, deionized water, HCl and NH3·H2The molar ratio of O is 0.4: 0.6: 6: 5: 2 × 10-3：3×10-3。
Further, the alkoxy silane comprises one or two or more of methyl trimethoxy silane, methyl triethoxy silane, ethyl trimethoxy silane and dimethyl dimethoxy silane.
Further, the fiber comprises one or more of glass fiber, quartz fiber, ceramic fiber, carbon fiber, polyimide fiber and polyester fiber.
Further, the HCl solution added dropwise in step S1.1 has a concentration of 0.2 mol. L-1Step S2.1, the concentration of the dropwise added HCl solution is 0.1 mol-L-1。
Further, step S2.3 is that the molar ratio of ethyl orthosilicate to absolute ethyl alcohol in the mixed solution of ethyl orthosilicate and absolute ethyl alcohol is 2: 8.
Further, the normal-pressure grading drying operation of the step S2.4 is carried out in four stages, the temperature of the first-stage low-temperature drying is 60-70 ℃, and the drying time is 1-2 hours; the temperature of the secondary low-temperature drying is 80-90 ℃ and the drying time is 2-3 hours; the temperature of the third-stage heat treatment is 110-120 ℃ for 2-3 hours; the temperature of the four-stage heat treatment is 140-150 ℃, and the drying time is 1-2 hours.
Further, in the drying treatment process of the step S2.4, the mould is sealed by adopting a preservative film, a small number of needle holes are pricked on the surface of the preservative film by using needles, and then the preservative film is placed into a constant-temperature electrothermal blowing drying oven for drying.
The invention has the beneficial effects that:
SiO of the invention2The process of aerogel preparation comprises: firstly, obtaining alcohol gel which has a certain three-dimensional network structure and takes a solution as a dispersion medium by a sol-gel method; secondly, compounding specially processed chopped fibers to increase the mechanical strength of the gel; and (III) changing the solvent in the alcogel network structure into air through a drying process to obtain the aerogel.
(I) Sol-gel technique
Compared with the traditional preparation method, the sol-gel method has the biggest characteristic that a liquid chemical reagent or sol but not a powdery material is used as a reactant, and the liquid chemical reagent or sol is uniformly mixed in a liquid phase and reacts, so that a stable sol system is generated, and no precipitate is generated in the reaction process.
The invention takes Tetraethoxysilane (TEOS) and alkoxy silane as mixed precursors and deionized water (H)2O) as reactant, absolute ethyl alcohol (EtOH) as cosolvent, 0.1mol L-1HCl and 0.5 mol. L-1 NH3·H2And O is an acid-base catalyst, and the gel is obtained through hydrolysis and polycondensation.
The hydrolysis and polycondensation reaction of the prior tetraethoxysilane are carried out very slowly at room temperature, and can be completed within days or even tens of days. In order to promote the generation of alcohol gel, the invention adopts a room temperature hydrolysis reaction and a two-step catalysis mode of acid and alkali, so that the gel time is finally shortened to several hours.
The reaction process in the sol-gel process is very complicated, and hydrolysis and polycondensation reactions generally occur simultaneously. First of all, silicic acid monomers and SiO bonded by silicon-oxygen bonds2Colloidal small particles, gradually polymerized into larger particles through a large number of hydroxyl or alkoxy groups existing on the surface; then, with the further occurrence of hydrolysis and polycondensation reaction, the silicic acid monomers and the small colloidal particles are further crosslinked with each other, so that nano-scale clusters are formed; further connection occurs between the last clusters, thereby forming disorderDendritic gel with nanometer level three-dimensional network structure. Due to SiO2The solvent filling the spaces between the three-dimensional network structures in the wet gel is mainly alcohol, so the SiO in this case2Wet gels are also known as alcogels.
Preparation of SiO2The precursor of the aerogel can be selected from water glass, halogen salt of silicon, alkoxide of silicon, rice husk containing silicon, fly ash and the like. However, the selection of water glass, silicon halide salt, silicon-containing rice husk and fly ash and the like has the following three disadvantages: 1) the raw material itself contains impurities such as Na+、Cl-、SO4 2-Etc. are difficult to remove; 2) most of the products have no definite stoichiometric number, and chemical proportioning is not easy to realize; 3) the prepared aerogel has poor performances in the aspects of density, specific surface area, thermal conductivity and the like. The invention takes Tetraethoxysilane (TEOS) and alkoxy silane as mixed precursors, and can generate a stable and high-quality sol system.
(II) fiber reinforcement
The fiber surfaces of glass fiber, quartz fiber, ceramic fiber, carbon fiber, polyimide fiber, polyester fiber and the like are smooth, the whole fiber is rod-shaped, natural bending is little, fiber slurry which is not subjected to fiber cutting and dispersion treatment is difficult to distribute uniformly and disperse when being compounded with other materials, the flocculation problem is easy to generate, and the uniformity of the materials is influenced. Therefore, uniform dispersion of the fibers is an important prerequisite for compounding with other materials.
The invention adopts HCl solution to soak the chopped fiber for 1.5 to 2.5 hours to remove impurities such as oil stains on the surface of the fiber. And then soaking the chopped fibers in 1.0 mass percent of silane coupling agent aqueous solution for treatment, improving the dispersibility of the chopped fibers, and remarkably improving the tensile strength and the tearing strength of a finished product so as to enable the finished product to meet the condition of compounding fibers with materials.
(III) drying
There is a large amount of solvent around the framework of the wet gel, and to try to obtain an aerogel, the solvent needs to be removed while maintaining the framework structure. At present, the drying methods for preparing the aerogel mainly comprise supercritical drying, subcritical drying, freeze drying and the like.
The invention comprehensively analyzes the principle of gel shrinkage deformation in a constant-speed drying period, and adopts normal-pressure graded drying, thereby improving the gel network strength, improving the gel skeleton structure, reducing the pressure gradient and reducing or even eliminating the shrinkage deformation of the gel. In addition, after hydrophobic modification, solvent replacement operation is carried out for multiple times, so that capillary pressure is reduced, and collapse of a silicon aerogel structure caused by solvent volatilization in drying is avoided.
According to the invention, the silicon dioxide aerogel is doped with the modified chopped fibers, so that the mechanical properties of the aerogel are effectively improved, and the tensile strength, the impact resistance and other properties are improved; and (3) performing hydrophobic modification on the aged gel to obtain the high-transparency and high-toughness silicon dioxide aerogel.
Drawings
FIG. 1 is a schematic representation of a fiber reinforced SiO of the present invention2Schematic representation of aerogel contact angle with water.
FIG. 2 is a schematic representation of a fiber reinforced SiO of the present invention2SEM scanning electron micrograph of aerogel 100 μm.
FIG. 3 is a fiber reinforced SiO of the present invention2SEM scanning electron micrograph of aerogel 5 μm.
FIG. 4 is a fiber reinforced SiO of the present invention2SEM scanning electron micrograph of aerogel 1 μm.
FIG. 5 is a fiber reinforced SiO of the present invention2SEM scanning electron micrograph of aerogel 0.1 μm.
Detailed Description
The embodiments of the present application are further described below with reference to the following figures and specific examples:
a process for preparing the fibre-reinforced silicon dioxide aerogel uses TEOS and methyltrimethoxysilane (MTMS) as the mixed precursor and deionized water (H)2O) as reactant, absolute ethyl alcohol (EtOH) as cosolvent, 0.1mol L-1HCl and 0.5 mol. L-1 NH3·H2O is acid-base catalyst, 0.8 percent of fiber with the length of 1mm is added for SiO2The aerogel structure is reinforced, and the sol-gel-normal pressure drying method is adopted to prepare the fiber reinforced SiO2An aerogel. The optimized process conditions by orthogonal test are as follows: raw materials of ethyl orthosilicate, methyltrimethoxysilane and absolute ethyl alcohol are removedWater, HCl, NH3·H2The molar ratio of O is 0.4: 0.6: 6: 5: 2 × 10-3：3×10-3。
Specifically, the method comprises the following steps:
s1 pretreatment of fibers
S1.1, cutting short and removing slag
The method comprises the steps of immersing and washing chopped fibers with the average length of 1mm, which are obtained by shearing ceramic fibers with the length of 30-80 mm and the diameter of 3-5 mu m by a crusher, in water for a plurality of times, and then 0.2 mol-L-1Soaking in HCl solution for 1.5-2.5 hr to remove impurities such as oil stain on fiber surface.
S1.2, chemical modification
And soaking the chopped fibers in a silane coupling agent CG-550 aqueous solution with the mass fraction of 1.0%, treating for 6h, taking out and drying for later use.
S2 fiber-reinforced SiO by mixed precursor method2Aerogel preparation
S2.1, preparation of Sol
Adding tetraethoxysilane, methyltrimethoxysilane, absolute ethyl alcohol and deionized water into a beaker, uniformly stirring, and adding 0.1 mol/L-1Adjusting the pH value of the HCl solution to 3-4, and continuously stirring for 5h at 25-30 ℃ to fully hydrolyze the HCl solution to obtain the silica sol.
S2.1, preparation of fiber-reinforced gel
Adding the pretreated chopped fiber obtained in the step S1, quickly stirring and dispersing for 30min, and slowly adding 0.5mol L dropwise-1NH of (2)3·H2Continuously stirring for 10min, pouring into a cylindrical mold, sealing and standing to form alcogel; during the process, the mould can be inclined by 45 degrees, and the gel reaction can be judged to be finished if the alcogel does not flow.
S2.3, aging treatment
Soaking the alcohol gel in a mixed solution of tetraethoxysilane and absolute ethyl alcohol with a molar ratio of 2:8, and aging for 48 hours; then, carrying out solvent replacement, and soaking and washing the alcohol gel in n-hexane for 12h, wherein the n-hexane is replaced once every 6 h;
s2.4, drying by stages under normal pressure
The aged fiber gel is passed throughThe pressure grading drying method is characterized in that a mould is sealed by a preservative film, a small number of needle holes are pricked on the surface of the preservative film by a needle, and then the preservative film is placed into a constant-temperature electrothermal blowing drying oven for drying. Drying is carried out in four stages, and the hydrophobic fiber reinforced SiO is prepared by drying for 2h, 3h and 2h at the temperature of 60 ℃, 90 ℃, 120 ℃ and 150 ℃ in sequence respectively2An aerogel composite.
The fiber-reinforced silica aerogel of the present embodiment has a nano-porous network structure, uniform particle size and pore distribution, and ceramic fibers and SiO2The aerogel matrix is tightly combined and has certain elasticity. The silicon dioxide aerogel is doped with the modified chopped ceramic fibers, so that the mechanical property of the aerogel is effectively improved, the drying shrinkage of the ceramic fiber reinforced silicon dioxide aerogel is 4.06%, and the compressive strength (10% strain) is 118 KPa.
In addition, the addition of the MTMS precursor obviously improves the hydrophobicity of the gel, and the SiO is prepared from a single TEOS precursor by using the contact angle with water2The 67 ° of the aerogel was raised to 144 °, see fig. 1.
The above preferred embodiments should be considered as examples of the embodiments of the present application, and technical deductions, substitutions, improvements and the like similar to, similar to or based on the embodiments of the present application should be considered as the protection scope of the present patent.
Claims (8)
1. A preparation method of fiber reinforced silica aerogel is characterized by comprising the following steps:
s1 pretreatment of fibers
S1.1, cutting short and removing slag
Cutting the fiber with a crusher to obtain chopped fiber with the average length of 0.09-1.1mm, soaking in water for several times, and soaking in HCl solution for 1.5-2.5 h;
s1.2, chemical modification
Soaking the chopped fibers in 1.0 mass percent of silane coupling agent aqueous solution for treatment for 5-6h, taking out and drying for later use;
s2 fiber-reinforced SiO by mixed precursor method2Aerogel preparation
S2.1, preparation of Sol
Adding tetraethoxysilane, alkoxy silane, absolute ethyl alcohol and deionized water into a beaker, uniformly stirring, adding HCl solution, adjusting the pH to 3-4, and continuously stirring for 4-6h at 25-30 ℃ to perform full acid hydrolysis to obtain silicon dioxide sol;
s2.1, preparation of fiber-reinforced gel
Adding the chopped fibers pretreated in the step S1, and quickly stirring and dispersing; slowly dropping NH3·H2Continuously stirring the solution O uniformly, pouring the solution O into a mold, sealing and standing to form alcohol gel;
s2.3, aging treatment
Soaking the alcohol gel in a mixed solution of tetraethoxysilane and absolute ethyl alcohol, and aging for 48 hours; then, carrying out solvent replacement, and soaking and washing the alcohol gel in n-hexane for 12h, wherein the n-hexane is replaced once every 6 h;
s2.4, drying by stages under normal pressure
The aged fiber gel is subjected to normal pressure grading drying method to prepare hydrophobic fiber reinforced SiO2An aerogel composite.
2. The method for preparing a fiber-reinforced silica aerogel according to claim 1, wherein the mixture of tetraethoxysilane, alkoxysilane, absolute ethanol, deionized water, HCl, and NH3·H2The molar ratio of O is 0.4: 0.6: 6: 5: 2 × 10-3：3×10-3。
3. The method for preparing a fiber-reinforced silica aerogel according to claim 1, wherein the alkoxysilane comprises one or two or more of methyltrimethoxysilane, methyltriethoxysilane, ethyltrimethoxysilane, dimethyldimethoxysilane.
4. The method for preparing fiber reinforced silica aerogel according to claim 1, wherein the fiber comprises one or more of glass fiber, quartz fiber, ceramic fiber, carbon fiber, polyimide fiber, and polyester fiber.
5. The method for preparing a fiber-reinforced silica aerogel according to claim 1, wherein the HCl solution used in step S1.1 has a concentration of 0.2 mol-L-1Step S2.1, the concentration of the dropwise added HCl solution is 0.1 mol-L-1。
6. The method for preparing fiber-reinforced silica aerogel according to claim 1, wherein the molar ratio of the tetraethoxysilane to the absolute ethyl alcohol in the mixture of the tetraethoxysilane and the absolute ethyl alcohol in the step S2.3 is 2: 8.
7. The method for preparing fiber-reinforced silica aerogel according to claim 1, wherein the normal-pressure staged drying operation of step S2.4 is performed in four stages, the temperature of the primary low-temperature drying is 60 to 70 ℃, and the drying time is 1 to 2 hours; the temperature of the secondary low-temperature drying is 80-90 ℃ and the drying time is 2-3 hours; the temperature of the third-stage drying treatment is 110-120 ℃, and the time is 2-3 hours; the temperature of the four-stage drying treatment is 140-150 ℃, and the drying time is 1-2 hours.
8. The method for preparing fiber-reinforced silica aerogel according to claim 7, wherein the drying process of step S2.4 is drying.
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Cited By (7)
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| CN111848106A (en) * | 2020-07-30 | 2020-10-30 | 福建省中能泰丰节能环保科技有限公司 | High-temperature-resistant heat-insulating material and preparation method thereof |
| CN112745698A (en) * | 2020-12-29 | 2021-05-04 | 青岛华世洁环保科技有限公司 | Preparation method of modified aerogel, thermal insulation coating and application of modified aerogel |
| CN112851293A (en) * | 2021-02-04 | 2021-05-28 | 浙江岩谷科技有限公司 | Green heat-preservation heat-insulation sound-absorption composite material and preparation method thereof |
| CN113548817A (en) * | 2021-06-24 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method, product and application of aerogel composite material |
| CN114716229A (en) * | 2022-04-14 | 2022-07-08 | 中国科学技术大学先进技术研究院 | Silicon carbide aerogel and preparation method thereof |
| CN115849863A (en) * | 2022-11-23 | 2023-03-28 | 江苏朗耐德耐火材料有限公司 | Fire-resistant aerogel composite thermal insulation material and preparation method thereof |
| CN116469626A (en) * | 2023-03-15 | 2023-07-21 | 西安湄南生物科技股份有限公司 | Aerogel insulation panel and manufacturing method thereof |
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| CN112745698A (en) * | 2020-12-29 | 2021-05-04 | 青岛华世洁环保科技有限公司 | Preparation method of modified aerogel, thermal insulation coating and application of modified aerogel |
| CN112851293A (en) * | 2021-02-04 | 2021-05-28 | 浙江岩谷科技有限公司 | Green heat-preservation heat-insulation sound-absorption composite material and preparation method thereof |
| CN113548817A (en) * | 2021-06-24 | 2021-10-26 | 惠州锂威新能源科技有限公司 | Preparation method, product and application of aerogel composite material |
| CN114716229A (en) * | 2022-04-14 | 2022-07-08 | 中国科学技术大学先进技术研究院 | Silicon carbide aerogel and preparation method thereof |
| CN115849863A (en) * | 2022-11-23 | 2023-03-28 | 江苏朗耐德耐火材料有限公司 | Fire-resistant aerogel composite thermal insulation material and preparation method thereof |
| CN115849863B (en) * | 2022-11-23 | 2024-03-01 | 江苏朗耐德耐火材料有限公司 | Fireproof aerogel composite heat-insulating material and preparation method thereof |
| CN116469626A (en) * | 2023-03-15 | 2023-07-21 | 西安湄南生物科技股份有限公司 | Aerogel insulation panel and manufacturing method thereof |
| CN116469626B (en) * | 2023-03-15 | 2024-01-02 | 西安湄南生物科技股份有限公司 | Aerogel insulation panel |
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