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Preferred orientation growth method of MFI type zeolite

A technology of preferred orientation and growth method, which is applied in the field of preferred orientation growth of MFI zeolite, can solve the problems of high toxicity of template agents, and achieve the effects of avoiding environmental pollution, wide sources of raw materials, and good technical effects

Active Publication Date: 2013-01-16
CHINA PETROLEUM & CHEM CORP +1
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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 that there is a problem of high toxicity of the template agent in the prior art, and a new method for preferentially oriented growth of MFI type zeolite is provided

Method used

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  • Preferred orientation growth method of MFI type zeolite
  • Preferred orientation growth method of MFI type zeolite

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Experimental program
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Effect test

Embodiment 1

[0015] By 1SiO 2 : 0.01Al 2 o 3 : 0.41TEAOH: 0.31 acetylacetone: 31.76H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, then add ethyl orthosilicate dropwise, stir for 1 hour, then add acetylacetone, stir for 1 hour , adjusted to pH = 13.0 with 0.1N sodium hydroxide solution, and continued to stir for 5 hours. The obtained mixture was crystallized under hydrothermal conditions at 170°C for 4 days, washed, filtered and dried. The obtained product had the characteristic diffraction peak of MFI and preferentially grew in the (010) direction (b-axis).

[0016] XRD spectrum see figure 2 In the middle curve 1, the relative intensity of (020), (040), (060) and (080) peaks in the diffraction spectrum is significantly increased, which is obviously due to the preferred orientation of the MFI single crystal on the powder diffraction sample plate, and its (0h0) plane, That is, the cylindrical surface ...

Embodiment 2

[0018] By 1SiO 2 : 0.01Al 2 o 3 : 0.25TPAOH : 0.05 sodium oxalate : 32.0H 2 O Weigh each material, dissolve sodium aluminate in distilled water, add tetrapropylammonium hydroxide dropwise, stir for 1 hour, then add silica sol dropwise, stir for 1 hour, then add sodium oxalate, stir for 1 hour, use 0.1 N sodium hydroxide solution was used to adjust the pH to 12.0, and stirring was continued for another 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 200°C for 3 days, washed, filtered and dried. XRD spectrum see figure 2 In the middle curve 2, the relative intensity of (020), (040), (060) and (080) peaks in the same diffraction spectrum is obviously increased.

Embodiment 3

[0020] By 1SiO 2 : 0.02Al 2 o 3 : 0.23TEAOH: 0.278-hydroxyquinoline: 44.64H 2 O Weigh each material, dissolve aluminum triethoxide in distilled water, add tetraethylammonium hydroxide dropwise, stir for 1 hour, then add silica sol dropwise, stir for 1 hour, then add 8-hydroxyquinoline, stir for 1 hour , adjust pH=11.0 with 0.1N sodium hydroxide solution, and continue stirring for 5 hours. The resulting mixture was crystallized under hydrothermal conditions at 150°C for 6 days, washed, filtered and dried. XRD spectrum see figure 2 In the middle curve 3, the relative intensity of (020), (040), (060) and (080) peaks in the same diffraction spectrum is obviously increased.

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Abstract

The invention relates to a preferred orientation growth method of MFI type zeolite, and mainly solves the problem of high toxicity in conventional templates. The method comprises the following steps of mixing a silicon source, an aluminium source, a template R1, a template R2 and water; adjusting a pH value of the reaction mixture to 8-14 with an inorganic base; wherein the molar ratio in the reaction mixture is as follows: Al2O3 / SiO2=0-0.05, R1 / SiO2=0.1-2, H2O / / SiO2=10-100 and R2 / SiO2=0.05-2; and crystallizing the above mixture for 1-10 days at a temperature of 100-250 DEG C, separating, washing and drying the crystallized mixture, and thus the preferred orientation growth MFI type zeolite is obtained, wherein the template R1 is selected at least one from tetramethylammonium hydroxide pentahydrate, tetraethylammonium hydroxide, tetrapropylammonium hydroxide or tetrabutylammonium hydroxide; and R2 is selected at least one from beta-diketone, a beta-diketone salt, oxalic acid, oxalate, pyrocatechol or 8-hydroxyquinoline. The preferred orientation growth method solves the problem well, and can be used in industrial production of the MFI type zeolite.

Description

technical field [0001] The invention relates to a method for preferential and directional growth of MFI type zeolite. Background technique [0002] The pores of zeolite are the places where molecules come in and out during the process of adsorption and reaction. What affects the diffusion of molecules is the interaction between molecules and the zeolite framework, not the interaction between molecules themselves. The orientation of the crystal will greatly affect the diffusion path of molecules in the channel, mass transfer and heat transfer resistance, etc. There are two types of 10-membered ring channels in the MFI-type zeolite structure (see figure 1 ): One is an elliptical straight channel parallel to the b-axis direction, with a size of 0.56×0.54 nm; the other is a sinusoidal circular channel parallel to the a-axis direction, with a size of 0.51×0.54 nm. In this way, for MFI type zeolite, transport molecules can diffuse along these two types of pores, which will inevi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 李亚男金照生杨为民
Owner CHINA PETROLEUM & CHEM CORP
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