Method for rapidly synthesizing pure-phase small-grain ZSM-11 molecular sieve

A technology of ZSM-11 and small crystal grains, which is applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminosilicate zeolite, etc., can solve the problems of unfavorable industrial production and long crystallization time, and achieve the synthesis time Short, easy-to-handle, low-sodium effect

Active Publication Date: 2014-03-26
DATONG COAL MINE GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The problem with this method is that at low temperature crystallization (such as 100), the crystallization time is very long (23d); and at high temperature crystallization, it is easy to produce ZSM-5 molecular sieve heterocrystal or a-quartz phase
The above method has the disadvantage of long crystallization time, which is unfavorable for industrialized production

Method used

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  • Method for rapidly synthesizing pure-phase small-grain ZSM-11 molecular sieve
  • Method for rapidly synthesizing pure-phase small-grain ZSM-11 molecular sieve
  • Method for rapidly synthesizing pure-phase small-grain ZSM-11 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] First, dissolve 1.77 g of aluminum sulfate octadecahydrate in 120 g of deionized water, then add 10 g (30 wt %) of tetrabutylammonium hydroxide aqueous solution and 10.41 g of 1,8-octanediamine in sequence, stir until dissolved, and finally, under stirring, add 52.00 g silica sol solution (SiO 2 30wt%), after adding, continue to stir for 4h to make it evenly mixed, and the composition of the amount of substance of the reaction sol is Al 2 o 3 : SiO 2 : R1 : R2 : H 2 O=0.01: 1: 0.04: 0.28:35, R1 is tetrabutylammonium hydroxide, R2 is 1,8-octyldiamine. The above reaction sol was sealed in a 250 ml stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 160 °C for 1 day. Wash until neutral, dry overnight at 100°C to obtain the product, which is the crystal phase structure of ZSM-11 molecular sieve with pure phase and small crystal grains as tested by X-ray diffraction (XRD). The X-ray diffraction (XRD) diagram of the sample is shown in the ...

Embodiment 2

[0021] First, dissolve 0.89g of aluminum sulfate octadecahydrate in 100g of deionized water, then add 6.54g (30 wt%) tetrabutylammonium hydroxide aqueous solution and 8.78g of 1,8-octanediamine in sequence, stir until dissolved, and finally, under stirring , adding 52.00 g of silica sol solution (SiO 2 30wt%), after adding, continue to stir for 4h to make it evenly mixed, and the composition of the amount of substance of the reaction sol is Al 2 o 3 : SiO 2 : R1 : R2 : H 2 O=0.0050: 1 : 0.026 : 0.24 :30, R1 is tetrabutylammonium hydroxide, R2 is 1,8-octanediamine. The above reaction sol was sealed in a 250 ml stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 160 °C for 2 days. Wash until neutral, dry overnight at 100°C to obtain the product, which is the crystal phase structure of ZSM-11 molecular sieve with pure phase and small crystal grains as tested by X-ray diffraction (XRD). The X-ray diffraction (XRD) diagram of the sample is shown...

Embodiment 3

[0023] First, dissolve 0.51 g of sodium metaaluminate in 110 g of deionized water, then add 4 g (30 wt %) of tetrabutylammonium hydroxide aqueous solution and 9.41 g of 1,8-octyldiamine in sequence, stir until dissolved, and finally add 52.00 g of g silica sol solution (SiO 2 30wt%), after adding, continue to stir for 4h to make it evenly mixed, and the composition of the amount of substance of the reaction sol is Al 2 o 3 : SiO 2 : R1 : R2 : H 2 O=0.0125: 1 : 0.016 : 0.255 :31.9, R1 is tetrabutylammonium hydroxide, R2 is 1,8-octanediamine. The above reaction sol was sealed in a 250 ml stainless steel autoclave lined with polytetrafluoroethylene, and crystallized at 160 °C for 1 day. Wash until neutral, and dry at 100°C overnight to obtain the product. It is the crystal phase structure of the pure-phase small-grain ZSM-11 molecular sieve through X-ray diffraction (XRD). The X-ray diffraction (XRD) diagram of the sample is shown in the attached Figure 5 .

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Abstract

The invention discloses a method for rapidly synthesizing a pure-phase small-grain ZSM-11 molecular sieve. According to the method, the synthesis time is short, and the process is simple. Tetrabutyl ammonium hydroxide (R1) and 1, 8-diaminooctane (R2) are taken as composite template agents, a silicon source, an aluminum source, the template agents and water are uniformly mixed and prepared into synthetic sol, and the molar ratio of the synthetic sol is that Al2O3: SiO2: R1: R2: H2O is equal to (0.001-0.2): (0.001-1.0): (0.05-0.5): (10-100); and the mixture is subjected to hydrothermal crystallization for 1-2 days at the temperature of 160-190 DEG C, centrifugal separation, washing and drying are performed after cooling, and a pure-phase small-grain ZSM-11 molecular sieve sample is obtained. According to the method, tetrabutyl ammonium hydroxide and 1, 8-diaminooctane are taken as the composite template agents, a seed crystal is not required to be added to the synthetic sol, and the molecular sieve is rapidly synthesized at a high temperature. The method id short in synthesis time, simple in process and simple and convenient to operate; and the content of sodium in the synthesized ZSM-11 molecular sieve is low.

Description

technical field [0001] The invention discloses a method for rapidly synthesizing a pure-phase small-grain ZSM-11 molecular sieve, which belongs to the technical field of inorganic synthesis chemistry and catalytic application. Background technique [0002] ZSM-11 molecular sieve was first synthesized by Mobil Petroleum Company in the 1970s. Subsequent research found that ZSM-11 molecular sieves belong to the tetragonal crystal system, and ZSM-11 and ZSM-5 molecular sieves belong to the Pentasil family. The structural similarity of the two molecular sieves is that the secondary structural units have the same form of sheet structure; the difference is that the symmetry between adjacent secondary structural unit layers is different, and ZSM-5 conforms to the symmetry center correlation; ZSM-11 conforms to the mirror correlation, and has two-dimensional straight channels of ten-membered rings parallel to the a direction and the b direction, and the channel size is 0.54nm×0.53nm...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/36
Inventor 张海荣杨智文蒋煜郭万忠陶逊常晓华
Owner DATONG COAL MINE GRP
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