A kind of ultra-high transparency large-size bulk silica airgel and its preparation method and application
A technology of silica and transparency, applied in chemical instruments and methods, inorganic chemistry, silicon compounds, etc., to achieve high heat insulation performance, large economic benefits, and reduce energy consumption and heat loss
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[0034] In a first aspect, the present invention provides a method for preparing an ultrahigh-transparency large-size bulk silica aerogel, the method comprising the following steps:
[0035] (1) Silicon source methyl orthosilicate (TMOS silicon source), additive long-chain alkyl trimethoxysilane (C n TMOS), an alcohol solvent, water and an alkali catalyst are mixed uniformly and then hydrolyzed to obtain a sol, and then the sol is placed in a mold to perform a sol-gel reaction to obtain a wet gel;
[0036] (2) subjecting the wet gel to a gradient temperature aging step to obtain a skeleton-reinforced wet gel;
[0037] (3) Perform the steps of solvent replacement (such as solvent replacement in ethanol) and supercritical drying (such as supercritical carbon dioxide drying) of the skeleton-reinforced wet gel in sequence to obtain ultra-high transparency and large-size block silica gas gel.
[0038] The invention provides a method for preparing super-high transparency and large-...
Embodiment 1
[0061] ①Add 152g of methyl orthosilicate, 11.2g of octadecyltrimethoxysilane (additive) and 224g of methanol into a beaker, and stir mechanically at -20°C for 30min to obtain mixed solution A. Add 72g of deionized water and 710 μL of ammonia-methanol solution (concentration is 7mol / L) into the beaker, utilize mechanical stirring at room temperature for 3min, obtain mixed solution B (in this example, each component in the raw material is calculated by molar ratio of methyl orthosilicate Esters: Octadecyltrimethoxysilane: Methanol: Water: Ammonia (1:0.03:7:4:0.005). Add the mixed solution B to the mixed solution A drop by drop, and continue to maintain the hydrolysis reaction at -20°C for 90 minutes to obtain a sol; inject the above-mentioned cold sol close to the gel state into a detachable tetrafluoroethylene plate with an area of 16cm×16cm The sol-gel reaction was carried out in the mold at -20°C for 90 min to form a wet gel.
[0062] ②Put the above-mentioned flat mold wit...
Embodiment 2
[0067] Embodiment 2 is basically the same as Embodiment 1, the difference is:
[0068] In step ①, 152g of methyl orthosilicate, 3.73g of octadecyltrimethoxysilane and 64g of methanol were respectively added into the beaker, and stirred mechanically at -20°C for 30min to obtain a mixed solution A. Add 36g of deionized water and 426μL ammonia-methanol solution (concentration is 7mol / L) in the beaker, utilize mechanical stirring at room temperature for 3min, obtain mixed solution B (in this example, each component in the raw material is calculated by molar ratio of methyl orthosilicate Esters: Octadecyltrimethoxysilane: Methanol: Water: Ammonia (1:0.01:2:2:0.003). Add the mixed solution B to the mixed solution A drop by drop, and continue to maintain the hydrolysis reaction at -20°C for 90 minutes to obtain a sol. The above-mentioned cold sol close to the gel state is injected into a removable tetrafluoroethylene flat mold at -20°C The sol-gel reaction was carried out for 90 min...
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