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Preparation method of HZSM-5@SiO2 composite molecular sieve with high mesoporous degree

A composite molecular sieve, XZSM-5 technology, applied in molecular sieve catalysts, catalyst activation/preparation, chemical instruments and methods, etc., can solve problems such as difficult to control desiliconization rate, broken molecular sieve crystal structure, large mesopore diameter, etc., to promote Effects of diffusion and reactivity, inhibition of secondary isomerization reaction, and enhancement of shape-selective catalytic ability

Active Publication Date: 2020-10-13
LANZHOU UNIVERSITY OF TECHNOLOGY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, it is difficult to control the desilication rate by traditional alkali treatment using inorganic bases such as NaOH as alkaline reagents, which can easily lead to excessive desilication. Distributed mesoporous system; on the other hand, excessive desiliconization will cause serious damage to the skeleton structure, resulting in broken molecular sieve crystal structure, seriously affecting the catalytic effect (J.Mater.Chem.,2006,16(22):2121)

Method used

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  • Preparation method of HZSM-5@SiO2 composite molecular sieve with high mesoporous degree
  • Preparation method of HZSM-5@SiO2 composite molecular sieve with high mesoporous degree
  • Preparation method of HZSM-5@SiO2 composite molecular sieve with high mesoporous degree

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Experimental program
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Effect test

Embodiment 1

[0051] The high mesopority HZSM-5@SiO of this embodiment 2 The preparation method of composite molecular sieve, the method is:

[0052] S1. Mix 100mL of the alkali metal solution, the mixed solution of the pore-conducting agent PDAs, and 5g of HZSM-5 and stir to obtain a slurry;

[0053] Described alkali metal hydroxide solution is the sodium hydroxide solution that concentration is 0.1mol / L; Described guide hole agent PDAs is cationic surfactant TPA + ;

[0054] The cationic surfactant TPA + Molecular formula is N + (C 3 h 7 ) 4 , the structural formula is: where Na + and TPA + The molar ratio is 1:1;

[0055] S2. Stir the slurry obtained in S1 at a temperature of 80°C for 4 hours to form a gel mixture, then cool to room temperature, filter, wash with distilled water several times until neutral and dry, and obtain high mesopority NaZSM-5 molecular sieve;

[0056] S3, the high mesopority NaZSM-5 molecular sieve that obtains in S2 and the NH that concentration is 1...

Embodiment 2

[0087] The high mesopority HZSM-5@SiO of this embodiment 2 The preparation method of composite molecular sieve, the method is:

[0088] S1. Mix 100mL of the alkali metal solution, the mixed solution of the pore-conducting agent PDAs, and 2g of HZSM-5 and stir to obtain a slurry;

[0089] Described alkali metal hydroxide solution is that concentration is the sodium hydroxide solution of 1mol / L; Described hole guide agent PDAs is that anion surfactant is DS - ;

[0090] The anionic surfactant DS - The molecular formula is CH 3 (CH 2 ) 11 OSO 3 - , the structural formula is:

[0091] where Na + and DS - The molar ratio is 1:2;

[0092] S2. Stir the slurry obtained in S1 at a temperature of 50°C for 6 hours to form a gel mixture, then cool to room temperature, filter, wash with distilled water several times until neutral and dry, and obtain a high mesopority NaZSM-5 molecular sieve;

[0093] S3, the high mesopority NaZSM-5 molecular sieve that obtains in S2 and the ...

Embodiment 3

[0096] The high mesopority HZSM-5@SiO of this embodiment 2 The preparation method of composite molecular sieve, the method is:

[0097] S1. Mix 100mL of the alkali metal solution, the mixed solution of the pore-conducting agent PDAs, and 5g of HZSM-5 and stir to obtain a slurry;

[0098] Described alkali metal hydroxide solution is that concentration is the sodium hydroxide solution of 0.1mol / L; Described guide hole agent PDAs is that nonionic surfactant is EDA;

[0099] The molecular formula of the nonionic surfactant EDA is C 2 h 4 (NH 2 ) 2 , the structural formula is: where Na + The molar ratio with EDA is 2:3;

[0100] S2. Stir the slurry obtained in S1 at a temperature of 90°C for 2 hours to form a gel mixture, then cool to room temperature, filter, wash with distilled water several times until neutral and dry, and obtain high mesopority NaZSM-5 molecular sieve;

[0101] S3, the high mesopority NaZSM-5 molecular sieve that obtains in S2 and the NH that concentr...

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Abstract

The invention provides a preparation method of an HZSM-5@SiO2 composite molecular sieve with a high mesoporous degree. The method comprises the following steps of: mixing a mixed solution of an alkalimetal solution and a pore-guiding agent PDAs with HZSM-5 and then carrying out stirring to obtain slurry; conducting stirring to form a gel mixed solution; performing cooling, filtering, washing anddrying to obtain high-mesoporous-degree XZSM-5 molecular sieve; mixing the high-mesoporous-degree XZSM-5 molecular sieve with an NH4NO3 solution, carrying out ion exchange, and conducting drying and roasting for 2-3 hours to obtain a high-mesoporous-degree HZSM-5 molecular sieve seed crystal; and adding a dispersing agent and a silicon source, carrying out hydrothermal crystallization, and successively conducting washing, drying and roasting to obtain the high-mesoporous-degree HZSM-5@SiO2 composite molecular sieve. The high-mesoporous-degree HZSM-5@SiO2 composite molecular sieve prepared by the preparation method disclosed by the invention shows good catalytic performance and carbon deposition resistance in isomerization, alkylation and other reactions.

Description

technical field [0001] The invention belongs to the technical field of composite molecular sieve synthesis, in particular to a high mesopority HZSM-5@SiO 2 Preparation method of composite molecular sieve. Background technique [0002] HZSM-5 has a two-dimensional 10-membered ring channel, one of which is a 10-membered ring straight channel, and the other is a 10-membered ring channel with a Zigzag shape: the channel structure is [100] [010] Orthorhombic, Pnma, With its special pore structure, ZSM-5 molecular sieve not only provides a large number of access channels for reactants and products, but also provides good space restriction for shape-selective catalysis. [0003] HZSM-5 belongs to the orthorhombic molecular sieve with MFI structure (∣Na n (H 2 O) 16 ∣[Al n Si 96-n o 192 ]), the silicon-aluminum ratio can be from 10 until all-silicon Silicalite-1. The HZSM-5 molecular sieve structure contains strong acid sites (B acid) and weak acid sites (L acid), whi...

Claims

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Application Information

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IPC IPC(8): B01J29/40B01J37/04B01J37/30B01J37/08B01J37/10C01B39/38
CPCB01J29/40B01J37/04B01J37/30B01J37/08B01J37/10C01B39/38B01J2229/12Y02P20/52
Inventor 季东程春晖李红伟李贵贤
Owner LANZHOU UNIVERSITY OF TECHNOLOGY
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