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Synthesis method for ZSM-23 molecular sieve

A technology of ZSM-23 and molecular sieve, which is applied in the field of preparation route of HZSM-23 molecular sieve, can solve the problems of adding sodium exchange steps, increasing the difficulty of molecular sieve, increasing the production cost of molecular sieve, etc., and achieving the goal of simplifying the production process and reducing production cost Effect

Active Publication Date: 2013-01-30
CHINA PETROLEUM & CHEM CORP +1
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Problems solved by technology

[0005] In the existing research reports on the preparation of ZSM-23 molecular sieves, the synthesis system will contain alkali metal cations. The existence of these ions will increase the difficulty of the post-treatment of molecular sieves. For example, the presence of alkali metal cations will increase the sodium exchange step. , thereby increasing the production cost of molecular sieves

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  • Synthesis method for ZSM-23 molecular sieve

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preparation example Construction

[0013] The present invention provides a kind of preparation method of ZSM-23 molecular sieve, and this method comprises the following steps:

[0014] (1) Mix organic templating agent R with aluminum source, R and Al in the mixture 2 o 3 The molar ratio of the aluminum source is 0.2 to 20:1, the mixture is cooled in a closed reaction vessel at 50 to 190° C. for at least 0.1 hour to obtain an intermediate product, wherein the organic template R is isopropylamine and / or pyrrolidine;

[0015] (2) Mix and stir the intermediate product obtained in step (1) with silicon source, organic template, water and ZSM-23 seed crystals, and the final mixture molar ratio obtained is SiO 2 / Al 2 o 3 =20~200, R / SiO 2 =0.1~10,H 2 O / SiO 2 =3~20, said ZSM-23 seed crystal is based on SiO 2 0.5~15% by weight of the silicon source of mass meter, the amount of silicon oxide and aluminum oxide in the ZSM-23 seed crystal is not included in the molar proportion of said final mixture;

[0016] (3...

Embodiment 1

[0030] Take by weighing 3 grams of aluminum hydroxide (Beijing Chemical Plant, analytically pure, Al 2 o 3 content 35%), it is mixed with 8.4 grams of pyrrolidine aqueous solution (pyrrolidine content 70% by weight), and the ratio in the mixture is R / Al 2 o 3 =8 (molar ratio). It was placed in a crystallization kettle containing a polytetrafluoroethylene liner, cooled to room temperature after reacting at 150°C for 20 hours, after that, it was mixed with 40 grams of silica gel (Qingdao silica gel factory, SiO 2 content 98.4%), 81 grams of water, 8.3 grams of pyrrolidine and 2.4 grams of ZSM-23 seed crystals are fully mixed, and the molar ratio of the obtained mixture is: SiO 2 / Al 2 o 3 =65,H 2 O / SiO 2 =7, R / SiO 2 =0.3, the mixture was crystallized in an autoclave at 150° C. for 70 hours. After the crystallization, the molecular sieve is filtered, washed, dried at 120°C for 4 hours, and calcined at 550°C for 5 hours to obtain the hydrogen type molecular sieve.

[003...

Embodiment 2

[0033] Take by weighing 5 grams of pseudo-boehmite (Changling Catalyst Factory, Al 2 o 3 Content 75%), it is mixed with 24 grams of isopropylamine aqueous solution (isopropylamine content is 90% by weight), ratio is R / Al in the mixture 2 o 3=10 (molar ratio). It was placed in a crystallization kettle containing a polytetrafluoroethylene liner, cooled to room temperature after reacting for 30 hours at 130° C. 2 Content 98.4%), the mixture of 189 grams of isopropylamine, 804 grams of water and 22 grams of ZSM-23 seed crystals are fully mixed, the mixture molar ratio that obtains is: SiO 2 / Al 2 o 3 =120,H 2 O / SiO 2 =10, R / SiO 2 =0.8, the mixture was crystallized in an autoclave at 170° C. for 50 hours. After the crystallization, the molecular sieve is filtered, washed, dried at 120°C for 4 hours, and calcined at 550°C for 5 hours to obtain the hydrogen type molecular sieve.

[0034] According to XRD analysis, it has the same characteristics as the XRD spectrum of stand...

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Abstract

The present invention discloses a synthesis method for a ZSM-23 molecular sieve, comprising the steps of: mixing an organic templating agent and an aluminum source, and processing the mixture in a closed reactor at 50 DEG C to 190 DEG C for at least 0.1 hours then cooling to obtain an intermediate product, wherein the organic templating agent isopropylamine and / or pyrrolidine; mixing the intermediate product with a silicon source , organic templating agent, water and seed crystals uniformly, placing the obtained mixture in a closed reactor and processing for 15-72 hours at 130-180 DEG C, and obtaining a ZSM-23 molecular sieve product by recovering. According to the method, via changing introduction ways of the aluminum source, the presence of alkali metal cations in the synthetic reaction system is prevented, and a sodium ion exchange step is saved in the post-treatment process for the molecular sieve, simplifying the production process, and reducing the production cost.

Description

technical field [0001] The invention provides a preparation method of ZSM-23 molecular sieve, more precisely, a short-flow, low-cost preparation route of HZSM-23 molecular sieve. Background technique [0002] ZSM-23 molecular sieve is a medium-porous, high-silica molecular sieve with MTT topology. Its skeleton includes five-membered rings, six-membered rings and ten-membered rings. It is a one-dimensional channel molecular sieve. The ten-membered ring channel diameter is 0.56×0.45 nm. Due to its unique pore structure and suitable acidity, ZSM-23 molecular sieve has been used in many acidic catalysts, especially in butene isomerization and catalytic cracking reactions, such as the reaction of carbon tetraolefins to ethylene and propylene It has a good application prospect. [0003] The existing technical process for preparing molecular sieves is: synthesis-filtration-sodium exchange-drying-roasting. Judging from the existing patent literature reports, the main focus of wor...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 王殿中王萍冯强舒兴田何鸣元
Owner CHINA PETROLEUM & CHEM CORP
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