Process for producing silica aerogel
A silicon dioxide and aerogel technology, applied in the directions of silicon dioxide, silicon oxide, chemical instruments and methods, etc., can solve the problems of complex manufacturing process, product properties depend on molecular weight distribution, and reaction solution preparation takes a long time.
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[0024] The first method of producing silica airgel according to the present invention is characterized in that a silicon compound having a hydrolyzable functional group and a hydrophobic functional group in the molecule is added to a solution in which a surfactant is dissolved in an acidic aqueous solution, and hydrolyzed to form a gel. And after curing, the gel is supercritically dried.
[0025] A silicon compound having a hydrolyzable functional group and a hydrophobic functional group in the molecule is used as a starting material of the sol-gel method.
[0026] A substance having a hydrolyzable functional group and a hydrophobic functional group in a molecule shows affinity for a hydrophilic solvent and a hydrophobic solvent in a solution, respectively, and can form a fine phase-separated structure at the level of a mesoscopic mirror.
[0027] As the silicon compound, an alkyl silicon alkoxide is preferable. In particular, when a silica airgel is produced using methyltrime...
Embodiment 1
[0048] Mix 9.5 g of methyltrimethoxysilane (manufactured by Shin-Etsu Chemical Co., Ltd., LS-530, hereinafter abbreviated as "MTMS") and 5.0 g of nonionic surfactant, polyethylene glycol (10) nonyl Phenyl ether (manufactured by NOF Co., Ltd., NS210, hereinafter abbreviated as "NS210") was uniformly dissolved, and a 1 mol / L nitric acid aqueous solution was added to carry out a hydrolysis reaction while stirring the solution under ice cooling. Then, the mixture was stirred for 5 minutes under ice cooling while maintaining the above state. At this time, by changing the amount of nitric acid aqueous solution, MTMS:NS210:H 2 O=1:0.1:(1.8, 2.0, 2.2). They were then designated as MN21018, MN21020 and MN21022 according to the molar ratio of water added. Then, it was left to stand at 40°C in an airtight container for gelation. After gelation, the gel was aged by standing at 40° C. for 39 hours under airtight conditions. Next, the undried wet gel was immersed in 2-propanol for solve...
Embodiment 2
[0062] After mixing 1.819g of 1mol / L nitric acid aqueous solution, 7.315g of formamide and 5.0g of nonionic surfactant NS210 to make it dissolve uniformly, add 10.32g of tetramethoxysilane (Shin-Etsu Chemical Co., Ltd. Co., Ltd. product, LS-540, hereinafter abbreviated as "TMOS".) Hydrolysis reaction was carried out. Then, the mixture was stirred for 5 minutes under ice cooling while maintaining the above state. At this time, TMOS:formamide:H 2 The molar ratio of O is =1:2.4:1.4. This composition is referred to as "TF14". Then, it was left to stand at 40°C in an airtight container for gelation. After gelation, the gel was aged by standing at 80° C. for 48 hours under airtight conditions.
[0063] Then, a supercritical drying operation was performed in the same manner as in Example 1. The micropore diameter distribution of samples without cracks after supercritical drying was measured by mercury intrusion method. The result shown below is obtained. Scanning electron micr...
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