Aerogel precursor and aerogel produced by using same
A technology of airgel and precursor, applied in the field of airgel, can solve the problems of mechanical durability and other problems, achieve the effects of saving cost, improving high temperature thermal stability, and shortening the total process time
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[0022] Therefore, the present invention provides a method for preparing a hydrophobic airgel precursor, the preparation method comprising: preparing an alkoxysilane compound or a prehydrolyzed alkoxysilane compound; and adding a linear silane crosslinking agent to make the Alkoxysilane compounds or prehydrolyzed alkoxysilane compounds are polymerized wherein the linear silane crosslinker comprises units derived from PEG.
[0023] Hereinafter, the preparation method of the hydrophobic airgel precursor will be described in detail.
[0024] In the method for producing a hydrophobic airgel precursor of the present invention, an alkoxysilane compound or an alkoxysilane compound obtained by prehydrolyzing an alkoxysilane compound can be used as an airgel precursor.
[0025] Specifically, the alkoxysilane compound that can be used in the present invention can be selected from tetramethylorthosilicate (TMOS), tetraethylorthosilicate (TEOS), methyltriethylorthosilicate, orthosilicate ...
preparation Embodiment 1
[0061] Preparation Example 1: Preparation of prehydrolyzed alkoxysilane compound (alkoxydisiloxane prepolymer)
[0062] 150 g of TEOS, 51 g of ethanol, and 0.04 g of 35% aqueous HCl were added to a 500 mL reactor, and then stirred while raising the reaction temperature to 70°C. While the reaction temperature was kept at 70° C., 19.4 g of acidified distilled water containing 0.02 g of 35% aqueous hydrochloric acid solution was slowly added dropwise to the reactor over 1 hour, and then reacted for 8 hours.
[0063] After the reaction, the temperature of the reactor was cooled to room temperature. The cooled reactant was filtered using a filter under reduced pressure to remove impurities, thereby preparing a 75% hydrolyzed ethoxydisiloxane-based prepolymer (prehydrolyzed TEOS).
preparation Embodiment 2
[0064] Preparation Example 2: Preparation of linear silane crosslinkers comprising units derived from polyethylene glycol (PEG)
[0065] [Reaction 2]
[0066]
[0067] 19.79 g of isocyanate silane (KBE-9007, ShinEtsu Co., Japan), 12.80 g of polyethylene glycol PEG-400 (Korea, Deoksan Pure Chemicals Co., n=8.2 to 9.1) were added to a 1000 mL flask, and then 0.57 g of dibutyltin dilaurate (DBTDL) was added to make it 3 mole % relative to KBE-9007, and diluted with 300 g of tetrahydrofuran (THF) at room temperature to prepare a unit containing polyethylene glycol (PEG) linear silane crosslinkers. The mixture was stirred at room temperature until complete consumption of reactants was confirmed by thin layer chromatography (TLC), and then reduced pressure to remove all reaction solvents. Afterwards, under the developer solution condition of dichloromethane:methanol=30:1, 28 g of a liquid product with a purity of 95% or more was obtained by column chromatography, and the yiel...
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