US 12,479,967 B2
Thermally insulating aerogel vacuum composite panel and preparation method thereof
Ye Sun, Tianjin (CN); Pei Jiang, Tianjin (CN); Na Wu, Tianjin (CN); Jianwei Chen, Tianjin (CN); Peng Liu, Tianjin (CN); Fengxiang Bai, Tianjin (CN); Lianshan Han, Tianjin (CN); Jianlong Wang, Tianjin (CN); Jia Wang, Tianjin (CN); Dinghao Zhang, Tianjin (CN); and Dingxin Zhang, Tianjin (CN)
Assigned to Huabao (Tianjin) New MaterialScience And TechnologyDevelopment Co., Ltd., Tianjin (CN); and Shanxi Huabao New Materials Co., Ltd., Shanxi (CN)
Filed by Huabao (Tianjin) New Material Science And Technology Development Co., Ltd., Tianjin (CN); and Shanxi Huabao New Materials Co., Ltd., Shanxi (CN)
Filed on May 6, 2022, as Appl. No. 17/738,439.
Application 17/738,439 is a continuation of application No. PCT/CN2021/074129, filed on Jan. 28, 2021.
Prior Publication US 2022/0275164 A1, Sep. 1, 2022
Int. Cl. C01B 33/154 (2006.01); C08J 9/28 (2006.01); C08K 3/22 (2006.01); C08K 3/36 (2006.01); E04B 1/80 (2006.01); E04B 1/74 (2006.01)
CPC C08J 9/283 (2013.01) [C01B 33/154 (2013.01); C08K 3/22 (2013.01); C08K 3/36 (2013.01); E04B 1/803 (2013.01); C08J 2201/0504 (2013.01); C08J 2205/026 (2013.01); C08J 2383/04 (2013.01); C08K 2003/2227 (2013.01); E04B 2001/748 (2013.01)] 7 Claims
 
1. A preparation method of a thermally insulating aerogel vacuum composite panel, comprising the following steps:
(1) mixing tetraethyl orthosilicate (TEOS) solution having a mass concentration of 20-50% and a metal particle by a weight ratio of 100:(20-40), adding a hydrophobic agent having a mass concentration of 0.1-3%, mixing, and adding ammonium trifluoroacetate solution having a mass concentration of 0.1-5% dropwise until completely gelating to obtain a metal aerogel precursor, wherein a weight ratio of the TEOS solution to the hydrophobic agent is 100:(1-30);
(2) adding the metal aerogel precursor into an acid replacement solution with a mass concentration of 3-10% for replacement to obtain a gel, with a replacement temperature of 30-60° C. and a replacement time of 1-24 h;
(3) washing the gel obtained in step (2) with deionized water to obtain a neutral gel;
(4) soaking the neutral gel obtained in step (3) in a first organic resin solvent having a mass concentration of 0.1-5% for 4-8 h;
(5) homogenizing the gel obtained in step (4), pouring into a substrate with honeycomb structure, and aging for 4-8 h to obtain a modified panel;
(6) drying the modified panel obtained in step (5) to obtain a honeycomb panel; and
(7) aging the honeycomb panel obtained in step (6) at room temperature for 1-24 h under an absolute vacuum of 0.01-0.05 MPa;
wherein the modified panel obtained in step (5) is soaked in a second organic resin solvent having a mass concentration of 10-60%, replaced for 12-72 h, and dried;
wherein the modified panel obtained after replacing is sprayed with the deionized water until a white film appears on a surface of the modified panel to obtain a white surface modified panel.