Preparation method of FER (Ferritin) zeolite molecular sieve with high silica-alumina ratio

A technology of zeolite molecular sieve and high silicon-aluminum ratio, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve problems such as environmental pollution, narrow synthesis interval, waste of resources, etc., reduce production cost and environmental pollution, and improve the utilization of silicon rate, the effect of reducing the loss of silicon

Active Publication Date: 2013-07-17
EAST CHINA NORMAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the introduction of a large amount of organic templates in the above synthetic methods, a large amount of wastewater containing high-concentration templates will be produced in the zeolite molecular sieve washing process, which will cause a lot of pollution to the environment and waste of resources (Microporous and Mesoporous Materials 119 (2009) 60– 67; Phys. Chem. Chem. Phys., 2001, 3, 4164-4169; ACS Catal. 2013, 3, 617-621; Chemical Acta, 2003, 61, 835-839)
[0004] In addition to the introduction of structure-directing agents, many zeolite molecular sieve

Method used

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  • Preparation method of FER (Ferritin) zeolite molecular sieve with high silica-alumina ratio
  • Preparation method of FER (Ferritin) zeolite molecular sieve with high silica-alumina ratio

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] 2.59g CH 3 Add COOK and 1.59g NaOH solid to 80ml of deionized water, stir until the solution becomes clear, add 1.32g sodium metaaluminate to the above solution, and continue stirring at room temperature until the solid is completely dissolved. Add 13.8 g of fuming silica gel to the above mixed solution, continue to stir strongly magnetically for 1 hour, then add 1.38 g of FER zeolite molecular sieve into the reaction system as a seed crystal, continue stirring for 0.5 hour after the addition, and finally put the mixture into the poly In a tetrafluoroethylene-lined stainless steel crystallization kettle, airtightly crystallize in a microwave oven at 150 °C for 24 hours, and obtain a solid product after conventional suction filtration, washing, and drying. The molar composition of the initial sol of the mixture is: SiO 2 :Al 2 o 3 =30, Na 2 O:SiO 2 =0.25,H 2 O:SiO 2 =20.

[0024] The solid product is FER type zeolite through X-ray analysis, and finally obtained...

Embodiment 2

[0026] Except that column chromatography silica gel was used instead of the fumed silica gel in Example 1 as the silicon source, other preparation conditions were the same as in Example 1.

[0027] The solid product is analyzed as FER type zeolite by X-ray analysis, and the finally obtained FER sheet-shaped zeolite molecular sieve.

Embodiment 3

[0029] Except that Qingdao silica gel was used instead of the fumed silica gel in Example 1 as the silicon source, other preparation conditions were the same as in Example 1.

[0030] The solid product is analyzed as FER zeolite by X-ray analysis, and finally obtained FER flake zeolite molecular sieve has a silicon-aluminum ratio of 25.0.

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Abstract

The invention discloses a preparation method of an FER (Ferritin) zeolite molecular sieve with high silica-alumina ratio. The method comprises the following steps of: first, dissolving an aluminum source in a mixed liquid of sodium hydroxide, alkali and alkaline earth salt of weak acid; after adding the aluminum source, stirring and dispersing for a period of time by strong magnetic force at room temperature; mixing uniformly dispersed aluminum source and aluminum source liquid at room temperature to form glue; adding the FER zeolite molecular sieve as crystal seeds; after uniformly stirring and mixing at room temperature by strong force, transferring to a reaction crystallization kettle; crystallizing for 0.5-3 days by 130-170 DEG C microwave; and conventionally, filtering, washing and drying to obtain the sieve. According to the preparation method provided by the invention, expensive organic amine is not used as a structure-directing agent, and the FER zeolite molecular sieve is used as a crystal seed for microwave crystallization in an inorganic system with low alkalinity and high salinity. The crystallization degree and purity of products prepared are high, the silica-alumina ratio is easy to regulate, the synthetic cost is low, the environmental-pollution less, and the method is convenient for industrial large-scale production.

Description

technical field [0001] The invention relates to the synthesis of zeolite molecular sieves, in particular to a synthesis method of zeolite molecular sieves with FER topological structure. Specifically, without using an organic amine as a structure-directing agent system, by adding a seed crystal as a nucleation accelerator, in the presence of an alkali or an alkaline-earth metal inorganic salt, the synthetic route of using microwave heating is used to rapidly prepare a silicon-aluminum ratio modulation FER microporous zeolite molecular sieve. Background technique [0002] Ferrierite FER was originally a natural mineral, and ZSM-35 molecular sieve, which was first artificially synthesized by Plank et al. in 1977, is a kind of FER family. The structure of FER is a two-dimensional channel system composed of ten-membered rings of 0.438×0.55nm and eight-membered rings of 0.34×0.48nm. Due to the narrower pore free diameter and stronger surface acidity than ZSM-5, it has good cata...

Claims

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Application Information

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IPC IPC(8): C01B39/02
Inventor 张坤徐浪浪张三军宋正芳马晓静杨太群
Owner EAST CHINA NORMAL UNIV
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