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Preparation method of ITQ-24 zeolite molecular sieve

A technology of ITQ-24 and zeolite molecular sieves, which is applied in the field of synthesis of zeolite molecular sieves, can solve the problems of unstable structure of ITQ-24 molecular sieves, complex preparation of template agents, small molecular weight, etc., and achieves the advantages of easy promotion, low price, and cost-saving synthesis Effect

Active Publication Date: 2018-04-24
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The object of the present invention is to provide a kind of synthetic method of ITQ-24 molecular sieve in order to solve the problems such as complex preparation of the template agent used in the synthesis of ITQ-24 molecular sieve existing in the prior art, expensive cost, unstable structure of the obtained ITQ-24 molecular sieve, the method Synthesize ITQ-24 zeolite molecular sieve with simple, small molecular weight and cheap organic template, specifically, use choline hydroxide as template to synthesize ITQ-24 zeolite molecular sieve

Method used

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  • Preparation method of ITQ-24 zeolite molecular sieve
  • Preparation method of ITQ-24 zeolite molecular sieve

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Embodiment 1

[0022] Dissolve 1.046g of germanium oxide in 2.693g of 45wt% choline hydroxide aqueous solution, add 4.16g of tetraethylorthosilicate (TEOS) and 0.033g of aluminum isopropoxide, after the hydrolysis is complete, stir the container open overnight to volatilize ethanol , propanol and part of water until the reaction mixture reaches the final molar composition.

[0023] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170°C for crystallization for 168 hours. After the reaction, the solid was filtered, washed with distilled water, and dried at 100° C. to obtain a solid powder.

[0024] The obtained material was calcined as follows: the temperature was raised to 200°C within 30 minutes and kept at this temperature for 30 minutes, then the temperature was raised to 450°C within 60 minutes and kept at this temperature for 60 minutes, and finally the temperature was raised to 550°C within 30 minutes and held at this...

Embodiment 2

[0026] Dissolve 1.046g of germanium oxide in 2.693g of 45wt% choline hydroxide aqueous solution, add 4.16g of tetraethyl orthosilicate (TEOS) and 0.163g of aluminum isopropoxide, after the hydrolysis is complete, stir the container open overnight to volatilize ethanol , propanol and part of water until the reaction mixture reaches the final molar composition.

[0027] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170°C for crystallization for 168 hours. After the reaction, the solid is filtered, washed, dried and calcined to obtain the solid containing aluminum ITQ-24, and (Si+Ge) / Al=38 in the product.

Embodiment 3

[0029] Dissolve 1.046g of germanium oxide in 2.693g of 45wt% choline hydroxide aqueous solution, add 4.16g of tetraethyl orthosilicate (TEOS), after the hydrolysis is complete, open the container and stir overnight to volatilize ethanol and part of the water until the reaction mixture to reach the final molar composition.

[0030] The above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 170°C for crystallization for 168 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is ITQ-24 containing about 5% CDO molecular sieve impurity.

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Abstract

The invention relates to a synthesis method of an ITQ-24 zeolite molecular sieve, and mainly solves the problems of complicated preparation and high cost of organic template agents used for synthesizing an ITQ-24 zeolite molecular sieve and an unstable structure of the obtained ITQ-24 zeolite molecular sieve in the prior art. According to the invention, choline hydroxide which is low in price andcan be obtained from market sale is used as an organic template agent; a mixture is composed according to the following relationships: choline hydroxide / YO2=0.1-1.0, X2O3 / YO2=0-0.1, and H2O / YO2=1-30;hydrothermal crystallization is carried out on the mixture at 100-200 DEG C for 24-350 hours to obtain the porous crystalline zeolite molecular sieve material ITQ-24, wherein Y is at least one quadrivalent element, and X is at least one trivalent element. According to the invention, the cheap organic template agent is used, so that the synthesis cost is greatly reduced; the structure of the synthesized ITQ-24 molecular sieve is stable; and the method has a wide synthesis range, simple and feasible operation and convenient promotion.

Description

technical field [0001] The present invention relates to a kind of synthetic method of zeolite molecular sieve, relate to a kind of synthetic method of ITQ-24 zeolite molecular sieve more precisely. technical background [0002] Zeolite molecular sieves are crystalline porous silicate materials that are widely used as adsorbents, ion exchangers, and industrial catalysts. At present, there are 231 molecular sieve topologies approved by the International Molecular Sieve Association. [0003] Molecular sieves with multidimensional pore structures have diffusion advantages in catalytic reactions, and when the pores in each direction have different pore sizes, molecular sieves can exhibit unique shape-selective catalytic capabilities. From the perspective of petrochemical industry, molecular sieves with 12-membered ring × 10-membered ring channel structure have excellent catalytic performance in aromatic alkylation reactions. [0004] The topological structures of molecular siev...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/06C01B39/08B01J29/70
CPCB01J29/70C01B39/04C01B39/06C01B39/08C01P2002/72C01P2004/03
Inventor 付文华杨为民袁志庆滕加伟
Owner CHINA PETROLEUM & CHEM CORP
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