Phenolic resin/silicon dioxide composite aerogel materialand preparation method thereof

A composite airgel and silica technology, which is applied in the production of bulk chemicals, etc., can solve the problems of unavoidable phase separation, materials that cannot continue to maintain heat insulation and fire prevention, and fall off quickly, so as to achieve excellent heat insulation and fire prevention performance, and easy operation Simple, Response Safe and Reliable Effects

Active Publication Date: 2016-12-07
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
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Problems solved by technology

[0004] However, there is an important problem in the above methods, that is, the phase separation between the organic phase and the inorganic phase of the material cannot be avoided.
During the continuous combustion process, with the ablation of the organic phase, the inorganic phase will fall off rapidly due to the mesoscopic or macroscopic phase separation process between the two phases, so that the material cannot continue to maintain the performance of heat insulation and fire prevention

Method used

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  • Phenolic resin/silicon dioxide composite aerogel materialand preparation method thereof
  • Phenolic resin/silicon dioxide composite aerogel materialand preparation method thereof
  • Phenolic resin/silicon dioxide composite aerogel materialand preparation method thereof

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preparation example Construction

[0054] The present invention also provides a preparation method of phenolic resin / silicon dioxide composite airgel material, comprising the following steps:

[0055] a) In the presence of an acid, dispersing the organosilicon precursor and the phenolic compound in an aqueous solution, so that the organosilicon precursor is hydrolyzed to obtain a mixed solution;

[0056] b) mixing the mixed solution with chitosan, aldehyde compounds and water to form a sol, and then performing a hydrothermal reaction to obtain a phenolic resin / silicon dioxide composite hydrogel;

[0057] c) Drying the phenolic resin / silica composite hydrogel with supercritical carbon dioxide to obtain a phenolic resin / silica composite airgel material.

[0058] The preparation method provided by the present invention can prepare the above-mentioned phenolic resin / silicon dioxide double network airgel material with excellent heat insulation, fire prevention and ablation resistance. application in large-scale ind...

Embodiment 1

[0076] The present embodiment phenolic resin / silica double network aerogel is carried out as follows:

[0077]a. In a beaker with a volume of 50mL, add 15mL of water and 15mL of absolute ethanol, and add 1.882g of phenol, 6mL of tetraethyl orthosilicate and 0.6mL of glacial acetic acid, seal it, stir at room temperature for 24h, and perform hydrolysis to obtain The mixed solution is denoted as solution A;

[0078] B, in another beaker, 0.45g chitosan (Shanghai Sinopharm Group, CAS number: 9012-76-4) is dispersed in 15mL water, and gained chitosan solution is recorded as solution B;

[0079] Pour solution A into solution B quickly, and add 3mL formaldehyde solution (37wt% formaldehyde) to it, and continue to stir vigorously for 10min to form a sol;

[0080] The sol was packed into a 50mL polytetrafluoroethylene-lined hydrothermal reaction kettle, placed in an oven at 160°C, and hydrothermally reacted for 10h to obtain a yellow phenolic resin / silica double network composite hyd...

Embodiment 2

[0086] Utilize the preparation method identical with embodiment 1:

[0087] a. In a 50mL beaker, add 10mL of water and 20mL of absolute ethanol, and add 2.202g of resorcinol, 6mL of methyl orthosilicate and 0.6mL of glacial acetic acid, seal it, stir at room temperature for 24 hours, and perform hydrolysis , the resulting mixed solution is denoted as solution A;

[0088] B, in another beaker, 0.45g chitosan (Shanghai Sinopharm Group, CAS number: 9012-76-4) is dispersed in 15mL water, and gained chitosan solution is recorded as solution B;

[0089] Pour solution A into solution B quickly, and add 3mL formaldehyde solution (37wt% formaldehyde) to it, and continue to stir vigorously for 10min to form a sol;

[0090] The sol was packed into a 50mL polytetrafluoroethylene-lined hydrothermal reaction kettle, placed in an oven at 100°C, and subjected to a hydrothermal reaction for 10h to obtain a resorcinol-formaldehyde resin / silica double network composite hydrogel ( hybrid gel). ...

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Abstract

The invention provides a phenolic resin/silicon dioxide compositeaerogel material and a preparation method thereof. The phenolic resin/silicon dioxide composite aerogel material has a nano-grid structure in which a silicon dioxide phase and a resin phase are mutually tangled. The phenolic resin/silicon dioxide composite aerogel material is prepared from a material containing an organic silicon precursor, a phenolic compound, an aldehyde compound and chitosan by virtue of a sol-gel method and supercritical carbon dioxide. According to the composite aerogel material, an organic phase and an inorganic phase are respectively continuous nano-scale tangle structures and are integrated with the mechanical property of organic aerogel and the thermal insulation property and fire resistance of silicon dioxide aerogel; and after the composite gel material with a thickness of 1cm is impacted by the 1300-DEG C flame of a blast burner for over 30 minutes, the falling and the separation of the inorganic phase are not caused, and meanwhile, the temperature of a protected side does not exceed 300 DEG C. The preparation method has the beneficial effects that the operation is simple, the reaction is safe and reliable, and the thermal insulation property and the fire resistance of the material can be regulated and controlled by simply changing the material proportion.

Description

technical field [0001] The invention relates to the technical field of airgel materials, in particular to a phenolic resin / silicon dioxide composite airgel material and a preparation method thereof. Background technique [0002] Airgel material is a material with three-dimensional network structure and ultra-low density, which was first prepared by American scientist Kistler in 1931. Due to the unique three-dimensional structure and physical properties of airgel, it is widely used as a fireproof and heat insulating material in construction, aerospace and other high-tech fields. Currently reported aerogels with application prospects mainly include two types: 1. Inorganic aerogel materials represented by inorganic nano-units such as silica aerogel and graphene oxide aerogel; 2. Polyurethane Aerogels, phenolic resin aerogels, and epoxy resin aerogels are representative organic airgel materials. However, the fire performance of common organic aerogels cannot reach the level of...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L61/10C08L61/12C08L5/08C08K3/36C08J9/28C08G8/10C08G8/22
CPCC08G8/10C08G8/22C08J9/28C08J2361/06C08J2361/12C08J2405/08C08L61/06C08L61/12C08L2201/02C08L5/08C08K3/36Y02P20/54
Inventor 俞书宏于志龙杨宁
Owner UNIV OF SCI & TECH OF CHINA
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