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Clumpy hydrophobic phenolic resin/silicon dioxide compounded aerogel and preparation method thereof

A composite airgel and silica technology, which is applied in the field of bulk hydrophobic phenolic resin/silica composite airgel and its preparation, can solve the problems of difficulty in obtaining bulk materials, increasing costs, and prolonging production cycle. To achieve the effect of convenient industrial production, short production cycle and high safety

Inactive Publication Date: 2016-02-03
李永前
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The Chinese patents whose publication numbers are CN1803602A, CN101318659A, CN101671030A, and CN101973752A use fiber as a reinforcing phase through solvent replacement, surface hydrophobic treatment and fiber reinforcement process to obtain airgel composite materials under normal pressure drying, although these methods all use normal pressure drying , but there are still some deficiencies, which are manifested in that the prepared silica airgel is mainly powder, and it is difficult to obtain bulk materials; additional surface modification steps and solvent exchange steps are used, which prolong the production cycle and increase the cost

Method used

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  • Clumpy hydrophobic phenolic resin/silicon dioxide compounded aerogel and preparation method thereof
  • Clumpy hydrophobic phenolic resin/silicon dioxide compounded aerogel and preparation method thereof
  • Clumpy hydrophobic phenolic resin/silicon dioxide compounded aerogel and preparation method thereof

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preparation example Construction

[0035] The present invention also provides the preparation method of any above-mentioned massive hydrophobic phenolic resin / silicon dioxide composite airgel, and described method comprises the following steps:

[0036] (1) Mix a certain amount of phenols, aldehydes, aminosilanes, siloxanes with one or two hydrocarbon groups, distilled water and alcohols, and stir for 10-120 minutes to obtain a transparent sol; among them, phenols, aldehydes, The molar ratio of aminosilane, siloxane containing one or two hydrocarbon groups, distilled water, and alcohols is 1: (0.5-7.5): (0.1-3.5): (0.1-8.5): (1.5-45): (10 ~70), wherein the molar ratio of aminosilane is preferably 0.7~2.5, the molar ratio of distilled water is preferably 18~45, and the molar ratio of alcohols is preferably 20~50;

[0037] (2) The above-mentioned transparent sol is gelled, the gelation temperature is 20-95°C, preferably the gelation temperature is 60-70°C, and the gelation time is 1-20h to obtain a phenolic resin...

Embodiment 1

[0056] Mix 1.5g of phenol, 1.5g of formaldehyde, 2.5g of 3-aminopropyltrimethoxysilane, 3.0g of methyltrimethoxysilane, 5.0g of distilled water, and 20g of ethanol, and mix them thoroughly for 10 minutes to obtain a transparent sol, which gels at 50°C 10h to get a wet gel. The wet gel was dried for 48 hours under normal pressure at 50°C to obtain a phenolic resin / silica composite airgel. The density of the above-mentioned phenolic resin / silica composite airgel is 0.20 g cm -3 , porosity 88.2%, BET specific surface area 200m 2 g -1 , the contact angle between distilled water and the surface is 128°, the pore size distribution is 10-100nm, the elastic modulus is 5MPa, the compressive strength is 11.5MPa, and the thermal conductivity is 0.035W m -1 k -1 , the silica content is 35%. From figure 1 It can be seen from the figure that the composite airgel is a block, and the actual color is beige.

Embodiment 2

[0058] Mix 1.5g of phenol, 2.0g of formaldehyde, 2.5g of 3-aminopropyltrimethoxysilane, 3.5g of methyltriethoxysilane, 5.0g of distilled water, and 25g of ethanol, and mix them thoroughly for 50 minutes to obtain a transparent sol. Gel 5h to get wet gel. The wet gel was dried at 40°C under normal pressure for 48 hours to obtain a phenolic resin / silica composite airgel. The density of the above-mentioned phenolic resin / silica composite airgel is 0.15g cm -3 , porosity 91.0%, BET specific surface area 570m 2 g -1 ,From figure 2 It can be seen that the contact angle between distilled water and the surface is 138°, from image 3 and Figure 4 It can be seen that the pore size distribution is 7-120nm, the elastic modulus is 2MPa, the compressive strength is 3.5MPa, and the thermal conductivity is 0.03W m -1 k -1 , the silica content is 47%.

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Abstract

The invention relates to clumpy hydrophobic phenolic resin / silicon dioxide compounded aerogel and a preparation method thereof. The mass percentage content of silicon dioxide in the hydrophobic phenolic resin / silicon dioxide compounded aerogel is 10 to 70 percent; a porous structure performing a hydrophobic function is formed in the surface of the compounded aerogel; the contact angle between the surface of the compounded aerogel and water is 90 to 180 degrees. The clumpy hydrophobic phenolic resin / silicon dioxide compounded aerogel has the advantages that the lumping property and the porosity rate are high; the hydrophobic property is favorable; the mechanical strength reaches a certain extent; the thermal conductivity is low.

Description

technical field [0001] The invention belongs to the technical field of preparation of composite nanoporous materials, and in particular relates to a block hydrophobic phenolic resin / silicon dioxide composite airgel and a preparation method thereof. Background technique [0002] Silica airgel is a new material with a three-dimensional porous structure formed by stacking silica nanoparticles. Because of its low density (0.003~0.8g·cm -3 ), high porosity (80-99.8%), high specific surface area (200-1000m 2 g -1 ), low thermal conductivity (~0.02W·m -1 K -1 ) and other properties make it have very broad prospects in aerospace, chemical industry, energy-saving buildings, military, communications, electronics, metallurgy and other application fields. [0003] Although the research on aerogels has long been a hot spot for researchers, so far there are not many companies that have actually achieved commercial scale production and widely promoted applications. The main reason is...

Claims

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Application Information

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IPC IPC(8): C08L61/10C08L61/12C08L61/08C08K3/36C08J9/28C08J3/075
Inventor 李永前
Owner 李永前
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