US 11,866,612 B1
Preparation method of phosphate-based high-temperature-resistant adhesive self-reinforced by in-situ growth and locking of flaky kyanite
Haijun Zhang, Tianjin (CN); Mingchao Wang, Tianjin (CN); Qingsong Zhang, Tianjin (CN); Zhenyu Feng, Tianjin (CN); and Yu Wu, Tianjin (CN)
Assigned to Civil Aviation University of China, Tianjin (CN)
Filed by Civil Aviation Uhiversity of China, Tianjin (CN)
Filed on Jul. 7, 2023, as Appl. No. 18/348,359.
Claims priority of application No. 202210816108.2 (CN), filed on Jul. 12, 2022.
Int. Cl. C09J 1/00 (2006.01); C09J 7/35 (2018.01); C09J 7/10 (2018.01); C08K 3/38 (2006.01); C08K 3/24 (2006.01); C08K 3/32 (2006.01); C08K 3/22 (2006.01); C08K 3/36 (2006.01); C08K 9/02 (2006.01); C08K 3/34 (2006.01)
CPC C09J 1/00 (2013.01) [C08K 3/22 (2013.01); C08K 3/24 (2013.01); C08K 3/32 (2013.01); C08K 3/346 (2013.01); C08K 3/36 (2013.01); C08K 3/38 (2013.01); C08K 9/02 (2013.01); C09J 7/10 (2018.01); C09J 7/35 (2018.01); C08K 2003/2227 (2013.01); C08K 2003/321 (2013.01); C08K 2003/329 (2013.01); C09J 2400/10 (2013.01)] 8 Claims
OG exemplary drawing
 
1. A preparation method for a phosphate-based high-temperature-resistant adhesive self-reinforced by in-situ growth and locking of flaky kyanite applied in a temperature range of 700 degrees Celsius (° C.) to 1300° C., comprising following steps:
step 1, mixing bauxite:kaolin:boric acid:boron oxide according to a mass ratio of 3.35-4.85:8-9:1.5-2.25:1-1.5 to obtain a mixture, placing the mixture in a ball milling tank, adding absolute ethyl alcohol into the ball milling tank according to a solid-liquid ratio of 1:0.8-1.2, carrying out ball milling for 6-12 hours at 250-350 revolutions per minute (r/min) by using a ball mill to obtain a ball-milled mixture, taking out the ball-milled mixture for drying and grinding to obtain a modified filler;
step 2, diluting concentrated phosphoric acid with a mass fraction of 85 wt. % to a mass fraction of 40-50 wt. % to obtain diluted phosphoric acid, heating the diluted phosphoric acid to a temperature range of 70-85° C. in a water bath kettle with a cooling reflux device, and then rapidly pouring aluminum hydroxide powder with an aluminum-phosphorus molar ratio of 0.65-0.85 into the diluted phosphoric acid under a mechanical stirring at 500-650 r/min, followed by keeping the temperature range of 70-85° C., stirring for 1-2 hours at 750-850 r/min, and then stirring for 6-8 hours at 300-400 r/min, thereby obtaining a white adhesive slurry; and
step 3, adjusting the temperature range of the water bath kettle in the step 2 to 50-65° C., then mixing the modified filler in the step 1 into the white adhesive slurry in the step 2 according to a solid-liquid mass ratio of 1:4 to 1:6, and mixing silicon powder with a mass fraction of 3-7 wt. % of a total mass of the modified filler and the white adhesive slurry into the modified filler and the white adhesive slurry, and then alternately stirring for 8-12 hours with different speeds at a speed range of 300-700 r/min, thereby preparing the phosphate-based high-temperature-resistant adhesive self-reinforced by in-situ growth and locking of flaky kyanite.