Preparation method for nanometer ZSM-5 hierarchical-pore aggregate
A ZSM-5 and aggregate technology is applied in the field of preparation of nano ZSM-5 hierarchical porous aggregates, which can solve the problems of cumbersome preparation process, long crystallization time, and difficulty in industrialization, and achieves simple preparation method and reduced diffusion resistance. , high repeatability
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Embodiment 1
[0041] Synthetic method: Add 15g of water, 0.051g of aluminum sulfate octadecahydrate, and 12g of tetrapropylammonium hydroxide into the reaction kettle. After stirring evenly, slowly add 5g of silica sol with a mass fraction of 40% during the stirring process, and add Add 4.0 g of dichlorodimethylsilane (DMCS), add 1 g of sodium hydroxide, stir for 30 min, and age the gel at room temperature for 24 h. After that, it was crystallized at 180°C for 2 days under stirring at 150rpm, cooled to room temperature, washed with deionized water and centrifuged three times, and dried at 80°C for 12 hours to obtain the final product.
[0042] From the XRD spectrum of the product obtained in Example 1, it can be seen that the product has a characteristic diffraction peak of ZSM-5, and has a relatively high degree of crystallinity. From the SEM photo of the product obtained in Example 1, it can be seen that the sample presents a spherical shape, the particle size is 3 microns, and it is form...
Embodiment 2
[0044] Using the same conditions as in Example 1, after stirring evenly, slowly add 4g of silicon powder dropwise during the stirring process, add 4g of dichlorodimethylsilane, add 1g of sodium hydroxide, stir for 30min, and age the gel at room temperature for 24h. After that, it was crystallized at 180°C for 2 days under stirring at 150rpm, cooled to room temperature, washed with deionized water and centrifuged three times, and dried at 80°C for 12 hours to obtain the final product. According to the XRD characterization results of the sample, it can be seen that the product has the characteristic diffraction peak of ZSM-5. The SEM photo shows that the sample presents a spherical shape with a particle size of 4 microns, which is formed by accumulation of nanoparticles. Due to the accumulation effect, the aggregate has a pore size of 3-6nm mesoporous structure, nano ZSM-5 particle size is 120nm. The BET data of the product obtained in Example 2 shows that the sample has a micro...
Embodiment 3
[0046] Synthetic method: Add 15g of water, 0.016g of aluminum isopropoxide, and 9g of tetrapropylammonium hydroxide into the reaction kettle. After stirring evenly, slowly add 5g of silica sol with a mass fraction of 40% dropwise during the stirring process, and add 5g of Add sodium hydroxide to trimethylchlorosilane (TMCS), stir for 30 minutes, and age the gel at room temperature for 24 hours. After that, it was crystallized at 180°C for 2 days under stirring at 150rpm, cooled to room temperature, washed with deionized water and centrifuged three times, and dried at 80°C for 12 hours to obtain the final product. According to the XRD characterization results of the sample, it can be seen that the product has the characteristic diffraction peak of ZSM-5. The SEM photo shows that the sample presents a spherical shape with a particle size of 2 microns, which is formed by the accumulation of nanoparticles. Due to the accumulation effect, the aggregate has a pore size of 3-6nm meso...
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