Method for preparing zeolite material in perforation type of multilevel pore canals

A technology of zeolite materials and channels, which is applied in the field of preparation of zeolite materials, can solve the problems of non-penetration, uniformity of zeolite, loading, etc., and achieve the effect of low device requirements, easy external control, and high specific surface area

Active Publication Date: 2007-07-25
CHINA PETROLEUM & CHEM CORP +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] Tang Yi et al. (CN 01126842.5) used diatomite as a carrier, formed a zeolite film on its surface through the nano-zeolite seed crystal layer-by-layer assembly method, and then grew it secondary under an organic amine atmosphere, thus forming a zeolite film on the diatomite. Zeolite material with a certain strength and multi-level pore structure, but the pores of zeolized diatomite are not interconnected, which will limit the diffusion
[0006] Hiroko Shikata et al. used the sol-gel method to load Silicalit-1 on a multi-level porous silica gel material (Journal of Sol-Gel Science and Technology, 19, 769-773, 2000), and later Takahashi et al. (EP 1 934 113 A2) used the vapor phase method to load Silicalit-1 and ZSM-5 zeolite in-situ on the hierarchical porous silica gel material, but these two loading methods could not make the zeolite evenly loaded on the hierarchical porous silica gel material. On flow-type silica gel materials, the size of zeolite grain growth cannot be effectively controlled, and the skeleton of part of the multi-stage channel through-flow silica gel material is destroyed during the preparation process.

Method used

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  • Method for preparing zeolite material in perforation type of multilevel pore canals
  • Method for preparing zeolite material in perforation type of multilevel pore canals
  • Method for preparing zeolite material in perforation type of multilevel pore canals

Examples

Experimental program
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Effect test

Embodiment 1

[0043] This example illustrates the process of using methyl orthosilicate as the silicon source to prepare a through-flow silica gel monolithic column with multi-stage channels.

[0044] Stir 30ml of methyl orthosilicate, 6g of polyethylene glycol and 30ml of 0.01mol / L acetic acid solution evenly, seal it, and stir at 0°C for 50min. The obtained sol was poured into a polytetrafluoroethylene test tube or a glass tube, and aged in a water bath at 30°C for one day to obtain a wet silica gel column. Then soak the silica gel column with 0.01mol / L ammonia water to prepare mesopores. Then soak the cylinder with 0.1mol / L nitric acid solution, distilled water, 30% ethanol / water ethanol solution and Tween 80 for 6 hours. Finally, dry and roast to obtain the multi-stage channel through-flow silica gel monolith material A 1 .

[0045] A 1 The SEM image is shown in Fig. 1, N 2 The adsorption-desorption curve is shown in Figure 12.

Embodiment 2

[0047] This example illustrates the process of preparing a through-flow monolithic column of silica gel with multi-stage channels using water glass solution as a silicon source.

[0048] Mix 20g of water glass solution, 2g of polyvinyl alcohol and 15ml of concentrated nitric acid evenly, pour the resulting sol into a test tube and seal it, place it in a water bath at 40°C for 40 hours, then soak it in deionized water for 4 days, and replace it every 24 hours. Water once, dry and roast at the end Multi-stage channel through-flow type silica gel monolithic material B 1 .

[0049] B 1 The SEM image is shown in Figure 2.

Embodiment 3

[0051] This example illustrates the process of preparing a double-hole silica gel column according to the method of Chinese Patent Application No. 200510073092.7.

[0052] Weigh 4.9737g of polyethylene glycol and pour it into a conical flask, add 52ml of 0.01mol / L acetic acid, and stir until completely dissolved. Measure 28.4ml TMOS into the conical flask, place the conical flask in an ice-water bath and stir vigorously for 30 minutes, then pour the obtained sol into a glass tube and seal it, and place it in a water bath at 40°C for 1-2 hours to gel. Then the wet silica gel column was soaked in water-ethanol solution and kept at 60°C for 24h. Then soak in the ethanol solution of TMOS and keep at 70°C for 72h. Then wash the silica gel column with ethanol and n-heptane at 50°C for 24 hours respectively, and finally dry and roast to obtain the double-hole silica gel column sample C with enhanced hardness. 1 . C 1 In the shape of cylindrical particles with a height of 1 cm and...

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Abstract

This invention discloses a method for preparing multi-level porous cross-flow zeolite material. The method comprises: (1) dispersing zeolite microcrystal in water or inorganic salt solution to form colloidal solution; (2) soaking the multi-level porous cross-flow silica gel material in polyelectrolyte solution so that the surface of the modified backbone is charged; (3) soaking and washing the silica gel material obtained in step 2 in the colloidal solution obtained in step 1 under normal or negative pressure; (4) soaking the silica gel material obtained in step 3in the colloidal solution obtained in step 1 under normal or negative pressure, and performing secondary crystallization by using vapor phase method. The obtained multi-level porous cross-flow property and abundant macropores with high uniformity, and can be used in catalysis and adsorption-separation. It has obvious advantages against normal zeolite molecular sieve on catalyst, adsorbent, separating agent and water treatment.

Description

technical field [0001] The present invention relates to a preparation method of a zeolite material, and more particularly relates to a preparation method of a multi-stage channel through-flow zeolite material. Background technique [0002] As an inorganic porous material, zeolite has abundant micropores, molecular sieve selectivity and good thermal and hydrothermal stability, and is widely used in catalysis and separation processes. At present, the general preparation method of zeolite catalyst is: firstly crystallize a certain ratio of reactant material gel mixture at high temperature to obtain zeolite, then combine zeolite with a carrier with or without binder, and then form a finished catalyst product. In this way, the active component of the catalyst, zeolite, is dispersed in various parts of the catalyst body phase, but cannot be highly dispersed on the surface of the catalyst to fully exert its catalytic effect, and the diffusion limitation is introduced. In order to ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02C01B39/38C01B39/14C01B39/22C01B39/24
Inventor 赵天波雷骞宗保宁王艳芬童扬传
Owner CHINA PETROLEUM & CHEM CORP
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