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Nano-cluster assembled microporous-mesoporous composite molecular sieve and synthetic method thereof

A composite molecular sieve and synthesis method technology, applied in the field of molecular sieves and their preparation, can solve the problems of lower production costs, poor thermal and hydrothermal stability, and restricted applications, and achieve the effects of simple preparation methods, broad application prospects, and uniform size distribution

Inactive Publication Date: 2013-12-11
YANSHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the amorphous nature of the pore walls of mesoporous molecular sieves makes them weakly acidic and poor in thermal and hydrothermal stability, which limits the wide application of mesoporous molecular sieves.
Microporous molecular sieve ZSM-5, due to its uniform and well-developed microporous structure, high hydrothermal stability and strong acidity, shows good catalytic activity in industry, especially ZSM-5 synthesized by direct method greatly reduces production However, its small pore size restricts its application in the catalytic conversion of macromolecular heavy oil, residual oil, and some acid-catalyzed reactions controlled by diffusion

Method used

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  • Nano-cluster assembled microporous-mesoporous composite molecular sieve and synthetic method thereof
  • Nano-cluster assembled microporous-mesoporous composite molecular sieve and synthetic method thereof
  • Nano-cluster assembled microporous-mesoporous composite molecular sieve and synthetic method thereof

Examples

Experimental program
Comparison scheme
Effect test

example 1

[0030] Dissolve 0.24g of solid sodium hydroxide with 14.95g of deionized water, then add 0.26g of sodium metaaluminate and 2.12g of TPABr into the lye, stir well, then add 9.36g of silica sol (in the form of SiO 2 Then add 0.135g of Trixton X-100, stir the mixture at room temperature for 1.0h, and cultivate it at 140°C for 16h to obtain ZSM-5 molecular sieve nanocrystal clusters; figure 1 As shown, it can be seen from the figure that the ZSM-5 molecular sieve is spherical, and the particle size is about 5-6 μm.

[0031] Dissolve 2.71g of P123 in 17.53g of deionized water, stir in a constant temperature water bath at 35°C for 2h to make it a transparent colloidal solution; then add 5.80g of n-butanol (n-BuOH), and continue stirring for 1.0h to obtain a mesoporous template solution.

[0032] Slowly and evenly add the ZSM-5 nanocrystal clusters obtained in step 1 to the mesoporous template solution obtained above, and control the molar ratio of the materials to be Na 2 O: Al 2...

example 2

[0035] Dissolve 0.31g of solid sodium hydroxide with 16.66g of deionized water, then dissolve 0.49g of Al 2 (SO 4 ) 3 18H 2 O and 4.99g TPABr were added to the lye, and after stirring evenly, 7.65g tetraethyl orthosilicate TEOS (based on SiO 2 Add 0.60g of fatty alcohol polyoxyethylene ether AEO-9, stir the mixture at room temperature for 0.5h, and incubate at 170°C crystallization temperature for 2.0h to obtain ZSM-5 molecular sieve nanocrystal clusters, such as Further prolonging the crystallization time to 72h, can obtain as Figure 5 The ZSM-5 molecular sieve shown. from Figure 5 It can be seen that the ZSM-5 molecular sieve grain size is about 1.8 μm, and the distribution is relatively uniform.

[0036]Dissolve 12.78g of P123 in 14.72g of deionized water, stir in a constant temperature water bath at 35°C for 2.0h to make it a transparent colloidal solution; then add 4.38g of n-butanol (n-BuOH), and continue stirring for 1.0h to obtain a mesoporous template agent s...

example 3

[0040] 0.23g solid sodium hydroxide was dissolved with 12.53g deionized water, then 0.07g KAlO 2 And 3.06g TPABr joins in the lye, after stirring evenly, add 8.77g water glass (as SiO 2 Then add 0.25g of alkylphenol polyoxyethylene ether OP-10, stir the mixture at room temperature for 3.0h, and incubate at 150°C crystallization temperature for 10h to obtain ZSM-5 molecular sieve nanocrystal clusters.

[0041] Dissolve 9.80g of P123 in 18.19g of deionized water, stir in a constant temperature water bath at 35°C for 2.0h to make it a transparent colloidal solution; then add 5.03g of n-butanol (n-BuOH), and continue stirring for 1.0h to obtain a mesoporous template agent solution.

[0042] Slowly and evenly add the ZSM-5 nanocrystal clusters obtained in step 1 to the mesoporous template solution obtained above, and control the molar ratio of the materials to be Na 2 O: Al 2 o 3 : SiO 2 :TPABr:H 2 O: P123: n-butanol=2.5:0.3:35:10:2400:1.5:60 Add 12.32g of 20% hydrochloric ac...

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Abstract

A nano-cluster assembled microporous-mesoporous composite molecular sieve is characterized in that the mesoporous phase of the composite molecular sieve is a three-dimensional cubic structure KIT-6 molecular sieve, and the microporous phase of the composite molecular sieve is a ZSM-5 molecular sieve. A preparation method of the composite molecular sieve comprises the following steps: mixing materials according to a certain mole ratio, adding a surfactant, stirring, and cultivating at a crystallization temperature of 140-170DEG C for 1-16h to obtain ZSM-5 molecular sieve clusters; dissolving a mesoporous template triblock copolymer in deionized water, stirring in a constant-temperature water bath to form a transparent colloidal solution, and adding n-butanol to obtain a mesoporous template solution; and adding the ZSM-5 molecular sieve clusters to the mesoporous template solution, stirring to obtain a gel, carrying out static crystallization of the gel, and roasting at 550DEG C for 3-7h to obtain the ZSM-5 / KIT-6 composite molecular sieve. The composite molecular sieve has the pore advantage of a mesoporous material and also has the high acidity and high hydrothermal stability of the mesoporous molecular sieve; and the method is simple to operate and has good repeatability.

Description

technical field [0001] The invention relates to a molecular sieve and a preparation method thereof. In particular, the molecular sieve used as a catalyst for hydrodesulfurization and adsorption desulfurization of oil products and its preparation method. Background technique [0002] Ryoo et al. added a certain amount of n-butanol to the P123 solution, and synthesized a mesoporous material KIT-6 with a three-dimensional cubic structure and large pore size in a weak acid system. Applications in the field of catalysis provide good conditions. However, the amorphousness of the pore walls of mesoporous molecular sieves makes them weak in acidity and poor in thermal and hydrothermal stability, which limits the wide application of mesoporous molecular sieves. Microporous molecular sieve ZSM-5, due to its uniform and well-developed microporous structure, high hydrothermal stability and strong acidity, shows good catalytic activity in industry, especially ZSM-5 synthesized by direc...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04C01B39/38
Inventor 霍全宋建争宋金凤陈培培李亚萍
Owner YANSHAN UNIV
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