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Synthesis method of ferrierite (FER) zeolite molecular sieve and obtained FER zeolite molecular sieve

A technology of zeolite molecular sieve and synthesis method, which is applied in the direction of crystalline aluminosilicate zeolite, iron conglomerate crystalline aluminum silicate zeolite, etc., can solve the problems of difficult crystallization, high price, long crystallization time, etc., and achieve low cost , short production process, high crystallinity and specific surface area

Inactive Publication Date: 2012-07-04
SHANGHAI SHANSHAN TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is to overcome the expensive organic template used in the synthesis of FER zeolite molecular sieve by hydrothermal crystallization method in the prior art, and the synthesis of FER zeolite molecular sieve with high silicon-aluminum ratio is prone to ZSM-5 and mercerization Zeolite and other miscellaneous crystal phases. At the same time, existing processes generally use seeds. If seeds are not used, crystallization will become difficult or the crystallization time will be very long. This provides a method that can effectively synthesize high-silicon aluminum Ratio, significantly reduce template cost, and do not use the synthetic method of FER zeolite molecular sieve of crystal seed and the obtained FER zeolite molecular sieve

Method used

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  • Synthesis method of ferrierite (FER) zeolite molecular sieve and obtained FER zeolite molecular sieve
  • Synthesis method of ferrierite (FER) zeolite molecular sieve and obtained FER zeolite molecular sieve
  • Synthesis method of ferrierite (FER) zeolite molecular sieve and obtained FER zeolite molecular sieve

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Experimental program
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Embodiment 1

[0041] The synthesis method of FER zeolite molecular sieve:

[0042] (1) Al in the aluminum source according to the molar ratio 2 o 3 : SiO in silicon source 2 : MOH in alkali source: isopropylamine: pyrrolidine: H 2 O is 0.04: 1: 0.06: 0.4: 0.2: 18 feed intake, described aluminum source is aluminum nitrate, described silicon source is silica sol, and described alkali source is sodium hydroxide; Aluminum nitrate and sodium hydroxide Dissolve in deionized water, add silica sol while stirring, continue to stir for 1 hour until completely dissolved and mix evenly, then add mixed template agent while stirring, continue stirring for 1 hour to obtain a raw material mixture;

[0043] (2) The raw material mixture was hydrothermally crystallized at 180° C. for 72 hours under the condition of dynamic stirring at 500 rpm;

[0044] (3) The product after hydrothermal crystallization is filtered, washed, dried, and then calcined at 550° C. for 10 hours in an air atmosphere to obtain a F...

Embodiment 2

[0055] The synthesis method of FER zeolite molecular sieve:

[0056] (1) Al in the aluminum source according to the molar ratio 2 o 3 : SiO in silicon source 2 : MOH in alkali source: isopropylamine: pyrrolidine: H 2 O is 0.02: 1: 0.06: 0.4: 0.2: 18 feed intake, described aluminum source is aluminum nitrate, described silicon source is silica sol, and described alkali source is sodium hydroxide; Aluminum nitrate and sodium hydroxide Dissolve in deionized water, add silica sol while stirring, continue to stir for 1 hour until completely dissolved and mix evenly, then add mixed template agent while stirring, continue stirring for 1 hour to obtain a raw material mixture;

[0057] (2) Under the condition of dynamic stirring at 600rpm, the raw material mixture was hydrothermally crystallized at 180°C for 72 hours;

[0058] (3) The product after hydrothermal crystallization is filtered, washed, dried, and then calcined at 550° C. for 10 hours in an air atmosphere to obtain a FER...

Embodiment 3

[0064] The synthesis method of FER zeolite molecular sieve:

[0065] (1) Al in the aluminum source according to the molar ratio 2 o 3 : SiO in silicon source 2 : MOH in alkali source: isopropylamine: hexamethyleneimine: H 2 O is 0.01: 1: 0.06: 0.8: 0.2: 20 feed intake, the described aluminum source is aluminum nitrate, the described silicon source is silica sol, and the described alkali source is sodium hydroxide; Aluminum nitrate and sodium hydroxide Dissolve in deionized water, add silica sol while stirring, continue to stir for 1 hour until completely dissolved and mix evenly, then add mixed template agent while stirring, continue stirring for 1 hour to obtain a raw material mixture;

[0066] (2) Under the condition of dynamic stirring at 600rpm, the raw material mixture was hydrothermally crystallized at 160°C for 72 hours;

[0067] (3) The product after hydrothermal crystallization is filtered, washed, dried, and then calcined at 600° C. for 10 hours in an air atmosph...

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Abstract

The invention discloses a synthesis method of a ferrierite (FER) zeolite molecular sieve and the obtained FER zeolite molecular sieve. The synthesis method comprises the following steps: (1) adding an alkali source, an aluminum source, a silicon source and a template agent into water in turn to obtain a raw material mixture, wherein the template agent contains isopropylamine and an organic template agent which is used for synthesizing the FER zeolite molecular sieve through the existing hydrothermal crystallization method; (2) performing hydrothermal crystallization on the raw material mixture; and (3) filtering the hydrothermal crystallization product, washing, drying and roasting. By adopting the method, the FER zeolite molecular sieve with high silica-alumina ratio and pure phase can be synthesized and the cost of the template agent can be significantly reduced; and the method has the advantages of short production flow and low pollution, and is especially beneficial to industrial production and application.

Description

technical field [0001] The invention relates to a synthesis method of FER zeolite molecular sieve and the obtained FER zeolite molecular sieve. Background technique [0002] Ferrierite FER is the original natural mineral. ZSM-35 molecular sieve, which was first artificially synthesized by Plank et al. in 1977, is one of the FER family. According to the XRD-derived spectra, ZSM-35, ZSM-21, ZSM-38, Fu-9 and ferrierite are indistinguishable and therefore considered to belong to the same zeolite family, the ferrierite group FER. The structural feature of FER zeolite molecular sieve is a two-dimensional pore structure composed of ten-membered rings of 0.43*0.55nm and eight-membered rings of 0.34*0.48nm. Compared with ZSM-5, it has a narrower pore free diameter and a smaller With strong surface acidity, it has great application potential in certain reactions such as n-butene isomerization to isobutene, xylene isomerization and CO hydrogenation to light olefins. [0003] The pre...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/44
Inventor 沈龙乔永民杜辉玉
Owner SHANGHAI SHANSHAN TECH CO LTD
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