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Preparation method of mesoporous ZSM-5 zeolite

A ZSM-5 and mesoporous technology, applied in the field of zeolite molecular sieve synthesis, can solve the problems of difficult industrial production acceptance, increased synthesis cost, and high synthesis cost, and achieve the effects of prolonging life, reducing diffusion resistance, and low synthesis cost

Active Publication Date: 2018-03-16
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the use of aminosilane and polyammonium group surfactants as mesoporous soft templates is expensive, and the synthesis cost is high, which is difficult to accept for industrial production, and the above synthesis methods all use tetrapropylammonium hydroxide (TPAOH) as microporous templates , tetraethyl orthosilicate (TEOS) is the silicon source, which further increases the synthesis cost

Method used

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  • Preparation method of mesoporous ZSM-5 zeolite
  • Preparation method of mesoporous ZSM-5 zeolite
  • Preparation method of mesoporous ZSM-5 zeolite

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 8.33g Al 2 (SO 4 ) 3 18H 2 O (chemically pure) was dissolved with 80g deionized, and then 8.82g concentrated sulfuric acid (98%) was added dropwise to prepare a uniform solution a; the molar ratio of solution a based on the following substances was: Al 2 o 3 :H 2 SO 4 :H 2 O=1:7:374. 100g water glass (SiO 2 ≥30wt%, modulus 3.5) mixed with 107g deionized water and 3g copolymer, stirred at room temperature for 1 hour, then slowly added solution a to the above solution under rapid stirring, and continued to stir for 6 hours to obtain a uniform gel. The molar ratio of described gel is based on the following substances: Na 2 O: SiO 2 :Al 2 o 3 :H 2 O=10:40:1:1120. The above gel was transferred to a high-pressure reactor and crystallized at 170°C for 110 hours. The crystallized product was filtered and washed until neutral, then dried at 120°C, and then calcined at 500°C for 8 hours to obtain a well-crystallized product. Mesoporous ZSM-5 zeolite. The specific ...

Embodiment 2

[0027] 5.55g Al 2 (SO 4 ) 3 18H 2 O was dissolved with 100g of deionized, and then added dropwise with 10g of concentrated sulfuric acid to prepare a uniform solution a; the molar ratio of solution a based on the following substances was: Al 2 o 3 :H 2 SO 4 :H 2 O=1:12:667. Mix 100g water glass with 105g deionized water and 4.5g copolymer, stir at room temperature for 2 hours, then slowly add solution a to the above solution under rapid stirring, and continue stirring for 5 hours to obtain a uniform gel. The molar ratio of described gel is based on the following substances: Na 2 O: SiO 2 :Al 2 o 3 :H 2 O=17:60:1:1800. The above gel was transferred to an autoclave for crystallization at 180°C for 72 hours, the crystallized product was filtered and washed until neutral, then dried at 110°C, and then calcined at 540°C for 8 hours to obtain a well-crystallized product Mesoporous ZSM-5 zeolite. The specific surface area of ​​the sample is 390.6m 2 / g, the micropore ...

Embodiment 3

[0029] 4.76g Al 2 (SO 4 ) 3 18H 2 O was dissolved with 120g deionized, and then 8.57g concentrated sulfuric acid was added dropwise to prepare a uniform solution a; the molar ratio of solution a based on the following substances was: Al 2 o 3 :H 2 SO 4 :H 2 O=1:12:933. Mix 100g water glass with 130g deionized water, 3.65g n-butylamine and 9g copolymer, stir at room temperature for 2 hours, then slowly add solution a to the above solution under rapid stirring, and continue stirring for 4 hours to obtain a uniform gel glue. The molar ratio of described gel is based on the following substances: Na 2 O: SiO 2 :Al 2 o 3 : NBA: H 2 O=19:70:1:7:2450. Transfer the above gel into an autoclave and crystallize at 175°C for 36 hours. The crystallized product is filtered and washed until neutral, then dried at 110°C, and then calcined at 540°C for 8 hours to obtain a well-crystallized product. Mesoporous ZSM-5 zeolite. The specific surface area of ​​the sample is 419.1m 2 ...

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Abstract

The invention discloses a preparation method of mesoporous ZSM-5 zeolite. The preparation method comprises the following steps: 1) allyl glycidyl ether and dimethyl diallyl ammonium are uniformly mixed, a sodium persulfate aqueous solution with mass concentration being 10-30% is added, the materials are uniformly stirred and heated to the temperature of 60-90 DEG C, and then a polymerization is carried out for 2-8 hours, and cooling is carried out to obtain a copolymer; 2) aluminum sulfate, concentrated sulfuric acid and deionized water are prepared to an uniform solution; 3) water glass, deionized water and the copolymer obtained in the step 1) are mixed, a mixture is continuously stirred for 0.5-3 hours, then the solution prepared in the step 2) is slowly added while rapid stirring, andthe materials are continuously stirred for 1-6 hours to obtain an uniform gel; and 4) the above gel is transferred to a high-pressure reaction vessel for crystallization, the crystallized products aresubjected to pumping filtration and washed to neutrality, and then the crystallized products are dried and roasted to obtain the mesoporous ZSM-5 zeolite. The prepared mesoporous ZSM-5 zeolite contains a lot of meso-structures, cost of raw material is low, operation is simple and easy, no special requirement is generated on equipment, and the method is suitable for industrial production and application.

Description

technical field [0001] The invention belongs to the field of zeolite molecular sieve synthesis, and relates to a method for preparing mesoporous ZSM-5 zeolite by a template method. Background technique [0002] ZSM-5 zeolite is a high-silica microporous zeolite with a three-dimensional intersecting channel system first synthesized by Mobil Corporation of the United States in 1972. Because of its good thermal stability, hydrothermal stability and shape-selective catalytic performance, it is widely used in the field of petrochemical industry. However, due to the small pore size of ZSM-5 zeolite (0.54 nm×0.56 nm), on the one hand, it is difficult for macromolecules to enter the pores; its scope of application. [0003] Recent studies have shown that introducing mesopores into microporous zeolite crystals can effectively improve the mass transfer efficiency and catalytic activity of zeolite materials for hydrocarbon molecules. Among them, the template method is an important p...

Claims

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Application Information

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IPC IPC(8): C01B39/40
CPCC01B39/40C01P2002/72C01P2006/12C01P2006/14C01P2006/17
Inventor 郑步梅王振宇方向晨郭蓉
Owner CHINA PETROLEUM & CHEM CORP
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