Preparation method of ddr zeolite molecular sieve

A technology of zeolite molecular sieve and synthesis method, which is applied in molecular sieves and alkali exchange compounds, chemical instruments and methods, crystalline aluminosilicate zeolite, etc. Mass diffusion is hindered, the method is efficient, and the operation is simple.

Active Publication Date: 2020-12-29
CHINA PETROLEUM & CHEM CORP +1
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The purpose of the present invention is to provide a synthetic method for DDR molecular sieves in order to solve the problems of expensive templates used in the synthesis of DDR molecular sieves in the prior art and the excessive crystal size of DDR molecular sieves

Method used

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  • Preparation method of ddr zeolite molecular sieve
  • Preparation method of ddr zeolite molecular sieve

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Experimental program
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Effect test

Embodiment 1

[0022] Dissolve 1.15g of boric acid and 0.45g of sodium hydroxide in 70g of water, add 19.9g of dimethyl diisopropylammonium hydroxide solution (20wt%) and stir evenly, and finally add 16ml of Ludox AS-40 silica sol slowly under stirring, After stirring for 1 h, the above mixture was put into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 160°C for crystallization for 120 hours. After the reaction, the solid was filtered, washed with distilled water, and dried at 100° C. to obtain a solid powder. The raw powder solid is placed in a muffle furnace and roasted at a temperature of 550° C. for 5 hours to obtain the final product. After calcination, the sample shows a stable DDR molecular sieve structure, and the XRD pattern is as follows figure 1 Shown; the primary particle size is 100-300nm, the aggregate size is 2-3μm, the SEM photo is as follows figure 2 shown.

Embodiment 2

[0024] Dissolve 1.15g of boric acid, 0.45g of sodium hydroxide, and 0.3g of aluminum isopropoxide in 70g of water, add 19.9g of dimethyl diisopropylammonium hydroxide solution (20wt%) and stir evenly, and finally slowly add 16ml of Ludox AS-40 silica sol, after stirring for 1 hour, put the above mixture into a crystallization kettle lined with polytetrafluoroethylene, and place it in an oven at 165°C for crystallization for 144 hours. The solid obtained after the reaction is filtered, washed, dried and calcined is DDR molecular sieve.

Embodiment 3

[0026] Dissolve 4g sodium tetraborate, 1.7g potassium hydroxide in 80g water, add 42g dimethyl diisopropyl ammonium hydroxide solution (20wt%) and stir evenly, finally slowly add 59g water glass (SiO 2 27wt%,Na 2 O 8.4 wt%), after stirring for 1 h, the above mixture was charged into a crystallization kettle with a polytetrafluoroethylene liner, and placed in an oven at 180° C. for 72 hours for crystallization. The solid obtained after the reaction is filtered, washed, dried and calcined is DDR molecular sieve.

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Abstract

The invention relates to a DDR zeolite molecular sieve synthesis method. In the prior art, the organic template for DDR zeolite molecular sieve synthesis is expensive and the crystal size of the DDR molecular sieve is too large. A purpose f the present invention is mainly to solve the problems in the prior art. According to the technical scheme, commercially available dimethyldiisopropylamine DMDIPA<+> is used as a templating agent, and a mixture is subjected to hydrothermal crystallization for 8-350 h at a temperature of 90-220 DEG C according to a ratio of DMDIPA<+> to YO2 to M2O to X2O3 toH2O of 0.05-1.0:1:0-0.75:0-0.1:1-100 to obtain a porous crystallized DDR zeolite molecular sieve material, wherein Y is at least a skeleton tetravalent element, X is at least a skeleton trivalent element, and M is an alkali metal element. According to the present invention, the cost of the used templating agent is low, the synthesized DDR zeolite molecular sieve has a small crystal grain size, andthe method has characteristics of simple operation, wide synthesis range and convenient promotion.

Description

technical field [0001] The present invention relates to a synthesis method of zeolite molecular sieve, more precisely relates to a synthesis method of DDR zeolite molecular sieve. [0002] technical background [0003] 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. [0004] The framework structure of DDR type zeolite molecular sieve is composed of [4] 3 5 8 6 1 ][5 12 ] and [4 3 5 12 6 1 8 3 ] and other three types of polyhedral structural units, the largest channel window consists of 8 TO 2 surrounded by tetrahedrons. The pore diameter of DDR molecular sieve is This is comparable to the diameter of many small molecule gases. Therefore, DDR molecular sieve is a kind of highly selective adsorbent, in the low carbon compounds such as CO 2 / CH 4 , Adsorptive...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/12C01B39/08C01B39/06
CPCC01B39/065C01B39/08C01B39/085C01B39/087C01B39/12C01P2002/72C01P2004/03C01P2004/61
Inventor 杨为民付文华袁志庆王振东滕加伟赵胜利
Owner CHINA PETROLEUM & CHEM CORP
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