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Preparation method of ZSM-5 mesoporous and microporous composite molecular sieve

A technology of ZSM-5 and composite molecular sieve, which is applied in the field of molecular sieves, can solve the problems of difficult industrialization, cumbersome technical steps, and small specific surface area, and achieve the effects of simplified synthesis steps, simple process, and large specific surface area

Inactive Publication Date: 2013-12-25
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

Zhu Y et al [Zhu Y, Hua Z, Zhou J, et al.Chemistry-A European Journal: Hierarchical Mesoporous Zeolites: Direct Self‐Assembly Synthesis in a Conventional Surfactant Solution by Kinetic Control over the Zeolite Seed Formation, 2011, 17( 51): 14618-14627] Utilizing TPAOH and CTAB as two templates, a hierarchical porous molecular sieve with a mesopore structure and a ZSM-5 micropore structure was prepared by nanometer self-assembly method, and the specific area of ​​the synthesized sample was Up to 440m 2 It has a concentrated 2.5nm pore size distribution. Compared with this technology, its specific surface area is small. At the same time, the 2.5nm pore size still cannot meet the needs of catalytic reactions involving many macromolecules.
Jiang Jianzhun et al [Jiang Jianzhun, Kang Yu, Zhang Mingsen. Advances in Chemical Industry: Preparation of ZSM-5 / MCM-41 Composite Molecular Sieve and Its Catalytic Activity for Ethanol Dehydration, 2012,31(1):112-116]Using NaOH solution to pretreat ZSM -5 molecular sieve, using hexadecyltrimethylammonium bromide as template agent, synthesized with a specific surface area of ​​600m 2 / g of ZSM-5 / MCM-41, but the technical steps are cumbersome and difficult to achieve industrialization

Method used

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  • Preparation method of ZSM-5 mesoporous and microporous composite molecular sieve
  • Preparation method of ZSM-5 mesoporous and microporous composite molecular sieve
  • Preparation method of ZSM-5 mesoporous and microporous composite molecular sieve

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Experimental program
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Embodiment 1

[0028] 0.328gNaAlO 2 and 15.589gTEOS (98%wt in H 2 O) Dissolve in 31.3g of water at 20°C and stir for 1h; gradually add 3.927g of TEAOH (25%wt in H 2 O) and stirred for 2h; put the mixed solution into a stainless steel high-pressure reactor, and react under homogeneous conditions at 90°C and 30r / min, and the reaction time is 1d; cool the reactor to room temperature, and drop it into the product at 60°C Add 0.486gCTAB and 96.7gH 2The mixed solution of O was stirred for 1 h; 12.593 g of EtOH was added dropwise to the mixture and stirred for 2 h; the mixed solution was put into a stainless steel autoclave, and crystallized at 140 ° C for 5 d; Extract the product by centrifugal filtration, put it in a vacuum drying oven and dry it at 40°C, put the dried product into a muffle furnace, set the ramp temperature rise to 2°C / min, calcinate at 500°C for 6h, and dry The final product can be directly put into the muffle furnace, and the initial temperature is in the room temperature ra...

Embodiment 2

[0030] 0.328gNaAlO 2 and 17.007gTEOS (98%wt in H 2 O) Dissolve in 19.3g of water at 20°C and stir for 1h; gradually add 4.712g of TEAOH (25%wt in H 2 O) and stirred for 2h; put the mixed solution into a stainless steel high-pressure reactor, and react under homogeneous conditions at 90°C and 30r / min, and the reaction time is 1d; cool the reactor to room temperature, and drop it into the product at 60°C Add 0.729gCTAB and 120.7gH 2 The mixed solution of O was stirred for 1h; 12.900g of EtOH was added dropwise to the mixture and stirred for 2h; the mixed solution was put into a stainless steel autoclave, and crystallized at 140°C for 5d; Extract the product by centrifugal filtration, put it into a vacuum drying oven and dry it at 40°C, put the dried product into a muffle furnace, set the ramp temperature rise to 2°C / min, and calcinate at 500°C for 6h to obtain a sample B2.

Embodiment 3

[0032] 0.328gNaAlO 2 and 15.589gTEOS (98%wt in H 2 O) Dissolve in 31.3g of water at 30°C and stir for 2h; gradually add 3.927g of TEAOH (25%wt in H 2 O) and stirred for 3h; the mixed solution was put into a stainless steel autoclave, and reacted under homogeneous conditions at 110°C and 40r / min, and the reaction time was 2d; the reactor was cooled to room temperature, and dripped into the product at 80°C Add 0.486gCTAB and 96.7gH 2 The mixed solution of O was stirred for 2h; 12.593g of EtOH was added dropwise to the mixture and stirred for 4h; the mixed solution was put into a stainless steel autoclave and crystallized at 160°C for 7d; Extract the product by centrifugal filtration, put it in a vacuum drying oven and dry it at 60°C, put the dried product into a muffle furnace, set the ramp temperature rise to 3°C / min, and calcinate it at 550°C for 7h to obtain a sample B3.

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Abstract

The invention discloses a preparation method of a ZSM-5 mesoporous and microporous composite molecular sieve. The method comprises the steps of dissolving NaAlO2 and TEOS (tetraethyl orthosili) in water, stirring to form a settled solution, dropwise adding TEAOH (tetraethylammonium hydroxide) into the settled solution, putting obtained mixed liquid in a high-pressure stainless steel reaction kettle for reaction under a homogeneous phase condition, cooling the reaction kettle to the room temperature, dropwise adding a mixed solution of CTAB (cetyltrimethyl ammonium bromide) and H2O into a product and stirring, dropwise adding EtOH (ethyl alcohol) and stirring, putting a product in the high-pressure stainless steel reaction kettle for hydrothermal synthesis reaction, repeatedly washing a product with water, centrifugally extracting, drying, placing a dried product in a muffle furnace for roasting, and obtaining the ZSM-5 mesoporous and microporous composite molecular sieve. The process of preparing the molecular sieve is simple; the method is good in repeatability; a synthesized material is provided with an excellent mesoporous and microporous composite duct structure; the mass transfer efficiency is improved during the reaction; therebfore, the method has better application prospects in macromolecular catalysis, adsorption, separated from and the like.

Description

technical field [0001] The invention relates to a molecular sieve, in particular to a method for preparing a ZSM-5 type medium-micro-double-hole composite molecular sieve, in particular to a method for preparing a ZSM-5 zeolite molecular sieve containing multi-stage channels of micropores and mesopores. Background technique [0002] Molecular sieves are widely used as catalysts in the petrochemical industry. They have excellent catalytic properties, such as uniform and developed microporous structure, high specific surface area, strong acidity and excellent hydrothermal stability. However, due to their The small pore size makes it difficult for macromolecules to enter the pores during the reaction process, and the mass transfer resistance is relatively large, which limits its application. Although mesoporous molecular sieves can make up for the lack of pore size of microporous molecular sieves, they are also difficult to be widely used because of their weak acidity and poor ...

Claims

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Application Information

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IPC IPC(8): C01B39/40
Inventor 奚红霞陈菲刘宝玉段倩倩葛敬辉
Owner SOUTH CHINA UNIV OF TECH
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