Silicon dioxide-based aerogel, composite material containing same, and preparation method and application of composite material

A silica and gel technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., can solve the problems of inability to obtain products with special complex structures, limit the application of silica aerogel, etc., and achieve high integrity , good mechanical properties, high specific surface area effect

Pending Publication Date: 2021-10-19
INST OF CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the harsh preparation process of silica and its hybrid aerogels makes the products of this material only suitable for the simplest molds, and it is impossible to obtain products with special complex structures, which limits the further application of silica aerogels

Method used

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  • Silicon dioxide-based aerogel, composite material containing same, and preparation method and application of composite material
  • Silicon dioxide-based aerogel, composite material containing same, and preparation method and application of composite material
  • Silicon dioxide-based aerogel, composite material containing same, and preparation method and application of composite material

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0068] A certain amount of tetraethyl orthosilicate (TEOS) was added dropwise to a mixed solution of absolute ethanol and 0.1 mol / L hydrochloric acid in an equimolar ratio, and magnetically stirred at room temperature for 24 hours to carry out sufficient acid-catalyzed hydrolysis condensation. After the reaction is completed, a certain proportion of coupling agent methacrylate propyl trimethoxysilane (MPTS) is added dropwise to the above solution, and magnetic stirring is continued at room temperature for 24 hours to form a resin solution. The configuration ratio and mass fraction of TEOS and MPTS in the above solution are given in Table 1:

[0069] Table 1

[0070]

[0071] Add 1wt% urotropine and 5wt% photoinitiator (2,4,6-trimethylbenzoyl) diphenylphosphine oxide to the above resin solution, stir until clear and transparent, then pour it into the photocuring 3D printer feed tank . Use the computer CAD software to export the three-dimensional structure model stl. format...

Embodiment 2

[0077] Follow V TEOS / V MPTS =23 / 7 ratio to prepare the resin solution, the solution preparation process and the photocuring 3D printing preparation process are the same as in Example 1. After the printing is completed, place the printed wet gel in the resin solution adding 1wt% urotropine, and place it under a light intensity of 20mW / cm 2 2-3 hours of light under the light source with a wavelength of 405nm. Then the obtained gel was packaged in a hydrothermal kettle and aged at 100°C for 3-4 days. The aged gel was subjected to 6 solvent replacements with absolute ethanol and n-hexane, and then the gel was hydrophobically modified with trimethylchlorosilane (TMCS), dried quickly under normal pressure, and the volume shrinkage was negligible. Complete airgel parts.

[0078] image 3 A-f in this example are the optical photos, SEM photos, TEM photos and EDS elemental analysis surface images of the photocured 3D printed silica-based airgel obtained in this example. image 3 I...

Embodiment 3

[0083] A sheet-like airgel with a thickness of 3 mm was prepared by printing according to Example 2. Fix the 3mm thick silica airgel with a metal bracket and place it horizontally above the flame to ensure that the outer flame of the flame touches the center of the bottom of the airgel, and perform an ablation test on it.

[0084] Figure 7 In the infrared thermal image shown in the figure, under the continuous 20s ablation of the outer flame at about 500°C, the 3mm thick 3D printed silica airgel showed good low conductivity and fire resistance; The temperature on the upper surface of the gel was only 96°C; when the flame left after 20s, the airgel did not continue to burn, and the surface temperature was only 140°C.

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Abstract

The invention discloses silicon dioxide-based aerogel with a complex structure, a composite material containing same, and a preparation method and application of the composite material. The framework of the silicon dioxide-based aerogel is formed by hybridizing and cross-linking a polyacrylate polymer and polysiloxane. Through a two-step method strategy, a hyperbranched silica chain is obtained under an acid catalysis condition and is modified with a silane coupling agent containing a photopolymerizable group, and then photocuring 3D printing is performed under an alkaline condition, so that the silicon dioxide-based aerogel which is high in complex structural integrity, high in specific surface area, good in mechanical property, capable of being rapidly dried at normal pressure and resistant to fire and flame is prepared. Meanwhile, an obtained silicon dioxide-based aerogel part with a three-dimensional complex structure is used as a reinforced framework, simple illumination is carried out after vacuum auxiliary solvent replacement to obtain the composite material with high transparency and high mechanical property, the macrostructure of the original aerogel is reserved, and the mechanical property of the polymer material in the field of photocuring 3D printing is effectively improved.

Description

technical field [0001] The invention belongs to the field of light-curing 3D printing materials, and in particular relates to a silica-based airgel material, a composite material thereof, a preparation method and application thereof. Background technique [0002] Silica airgel (SiO 2 aerogel) has been prepared by Kistler with supercritical drying technology since 1931. Due to its low density, high specific surface area, excellent heat insulation, good electrical insulation, adjustable transparency and fire resistance, it has always been an aerogel. The most studied and widely used class of gels. During these decades, a large number of researchers have adopted different strategies, such as polymer hybridization enhancement, coupling agent modification of the skeleton, etc. to obtain silica airgel with good integrity, normal pressure drying, and adjustable mechanical properties. . However, the harsh preparation process of silica and its hybrid aerogels makes the products o...

Claims

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Application Information

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IPC IPC(8): C01B33/158C08F222/14C08F2/44C08K7/26B33Y70/10
CPCC01B33/1585C08F222/102C08F2/44C08K7/26B33Y70/10C01P2004/64C01P2006/16C01P2006/14C01P2006/10C01P2006/12C01P2004/03C01P2004/04C01P2002/85C01P2002/88C01P2002/86C08F222/103
Inventor 邹为治钱振超徐坚赵宁
Owner INST OF CHEM CHINESE ACAD OF SCI
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