US 12,258,278 B1
Method for preparing organic-inorganic hierarchical ZSM-5
Yongfeng Zhang, Hohhot (CN); Zhifei Hao, Hohhot (CN); and Xingyuan Liu, Hohhot (CN)
Assigned to Inner Mongolia University of Technology, Hohhot (CN)
Filed by Inner Mongolia University of Technology, Hohhot (CN)
Filed on Aug. 28, 2024, as Appl. No. 18/817,272.
Claims priority of application No. 202311144799.7 (CN), filed on Sep. 6, 2023.
Int. Cl. C01B 39/38 (2006.01); B01J 20/16 (2006.01); B01J 20/30 (2006.01)
CPC C01B 39/38 (2013.01) [B01J 20/165 (2013.01); B01J 20/3021 (2013.01); B01J 20/3071 (2013.01); B01J 2220/46 (2013.01)] 4 Claims
 
1. A method for preparing an organic-inorganic hierarchical ZSM-5, comprising the following steps:
S1, mixing a silicon source, an aluminum source, NaOH, and a first water to obtain a first mixture, stirring the first mixture until uniformly dispersed, and drying and grinding the first mixture after uniformly dispersed to obtain a hierarchical ZSM-5 precursor, wherein a ratio of a part by amount (in mol) of a substance of silicon in the silicon source to a part by amount (in mol) of a substance of aluminum in the aluminum source, to a part by amount (in mol) of a substance of the NaOH, to a part by volume (in mL) of the first water is (20-80):(1-4):(0.5-2):(35-55);
S2, mixing the hierarchical ZSM-5 precursor, sodium silicate, a seed, ethanol, and a second water to obtain a second mixture, and uniformly dispersing the second mixture to obtain a crystallized solution, wherein in parts by mass, a ratio of the hierarchical ZSM-5 precursor to the sodium silicate to the seed to the ethanol and to the second water in the S2 is (1.5-3):(0.3-0.6):(0.06-0.12):(10-20):(30-60), wherein the seed is a ZSM-5 molecular sieve; and
S3, mixing the crystallized solution with a hydrolyzed organosilane to obtain a resulting solution, subjecting the resulting solution to a hydrothermal crystallization at 160-180° C. for 48-72 h to obtain a product, and washing and drying the product to obtain the organic-inorganic hierarchical ZSM-5, wherein in parts by mass, a ratio of the hydrolyzed organosilane to the hierarchical ZSM-5 precursor in the crystallized solution is (1-10):(1-7); and an organosilane is hexamethyldisilazane and/or methyltriethoxysilane, the hydrolyzed organosilane is obtained by hydrolyzing the organosilane for 2-4 h, and a method for obtaining the hydrolyzed organosilane comprises: mixing 0.5-3 parts by mass of the organosilane with 8-15 parts by volume of a third water to obtain a third mixture, and stirring the third mixture at 20-30° C. for 2-4 h, wherein a unit of the parts by mass is g, and a unit of the parts by volume is mL.