Hierarchical zeolite-based core/shell nano- or microcapsule
A technology of zeolite and hierarchical structure, which is applied in the directions of crystalline aluminosilicate zeolite, medical preparations containing active ingredients, borocarbonane silicone crystalline aluminosilicate zeolite, etc.
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Embodiment 1
[0110] (Synthesis of graded zeolites)
[0111] According to the method of Zhou et al. (“Synthesis of mesoporous ZSM-5zeolite crystals by conventional hydrothermal treatment.” RSC Advances 2013,3(36):15596-15599), mesoporous-ZSM-5zeolite crystals were synthesized as described in steps A to F below. 5.
[0112] A. Preparation of silicate solution: Tetraethyl orthosilicate (TEOS, 52g, USA), tetrapropylammonium hydroxide (TPAOH, 15.5mL 1M aqueous solution, 20%, ) and water (150 mL) were added to a polypropylene bottle, which was placed on a shaker for 24 hours to hydrolyze TEOS at room temperature and obtain a clear solution.
[0113] B. Preparation of aluminate solution: After about 22 hours of hydrolysis of TEOS in step A, aluminum isopropoxide (Al(O-i-Pr) 3, 2 g), NaOH (0.4 g in 10 ml of water), water (135 mL) and TPAOH (15.5 mL) were added to a glass beaker and stirred for about 2 hours until a clear aluminate solution formed.
[0114] C. Preparation of Synthesis Mixture...
Embodiment 2
[0119] (Characterization of the graded zeolite of Example 1)
[0120] Figure 5A and 5B SEM images of mesoporous-ZSM-5 before and after calcination are shown. Using energy dispersive x-ray spectroscopy (see Figure 6 ), the Si:Al weight ratio is determined to be Si:Al as 46.76:1.6. The XRD pattern of the synthesized mesoporous-ZSM-5 (see Figure 7 ) matched the simulated XRD pattern, which indicated that the synthesized particles were ZSM-5. Figure 8 Nitrogen adsorption-desorption isotherms of mesoporous-ZSM-5 are shown. The specific surface area is about 331m 2 / g. Figure 9 The pore size distribution of the as-synthesized ZSM-5 is shown. Based on BJH and HK calculations, it was determined that the mesopore size was about 4.96 nm and the micropore size was 0.64 nm, which meant that a graded zeolite was synthesized.
Embodiment 3
[0122] (Synthesis of MPS-modified mesoporous-ZSM-5)
[0123] Modification of Mesoporous-ZSM-5: Mesoporous-ZSM-5 (1 g) was dispersed in a mixture of ethanol (50 mL), water (5 mL) and aqueous ammonium solution (1 mL, 25%) by sonication for about 0.5 h . 3-(Methacryloyloxy)propyltrimethoxysilane (MPS, 2 mL) was added to the dispersion, and the reaction was continued for 72 hours with stirring. The resulting silica particles were then purified by three cycles of centrifugation, decantation and resuspension in ethanol in an ultrasonic bath. The modified mesoporous-ZSM-5 was dried in a vacuum oven at 60 °C to constant weight.
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