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Process for preparing multi-class sequential macroreticular-micropore material

A porous material and microporous technology, which is applied in the field of preparation of macroporous, microporous, and hierarchical ordered porous materials

Inactive Publication Date: 2002-04-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

How to organically combine macropores and micropores to solve this difficult production problem is a challenge for materials chemists

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0015] Example 1 First, zeolite A nanocrystals were prepared according to the method described in the literature (Thomas Bein et al, Science, 1999, 283, 958). The reaction ingredients are 0.3Na 2 O: 11.25 SiO 2 : 1.8 Al 2 o 3 : 13.4 (TMA) 2 O: 700H 2 O, the system uses 25% silica sol (pH=9) to replace 30% silica sol in the original literature, and the reported 97% tetramethylammonium hydroxide is replaced by 25% tetramethylammonium hydroxide aqueous solution. Specific process: adjust 25% silica sol (pH 9) to pH=10 with sodium hydroxide solution, accurately weigh 27g of the silica sol, add 15g of water, and stir to prepare precursor solution I. Simultaneously weigh 7.5g of aluminum isopropoxide, 100g of 25% tetramethylammonium hydroxide, 6g of 1M sodium hydroxide solution, and 25g of water, and stir to prepare precursor solution II. Finally, mix the two precursor solutions under vigorous stirring, stir and react at room temperature for one week, add flocculant-glucose 7.2...

Embodiment 2

[0019] Example 2 Zeolite X nanocrystals were prepared from silica sol, sodium aluminate, sodium hydroxide and water. The reaction process is as follows: 104g silica sol (25%SiO 2 ) (pH is 9), after cooling to 5° C., add 55 g of sodium hydroxide solution (50%), accurately weigh 27 g of the silica sol, add 78 g of water, and stir to make precursor solution I. Mix 61g of water, 30g of 50% sodium hydroxide solution and 20.36g of sodium aluminate (Al 2 o 3 43%), stirred to make precursor solution II. After adding 75g of crushed ice to each flooding solution, the two flooding solutions were mixed rapidly under vigorous stirring, and left for five minutes to form a gel. 22.5g of sucrose was added to the gel, and aged for 16 hours with stirring at room temperature. Dynamic hydrothermal reaction at 100°C for 2-4 hours, after repeated washing with water, a white final product was obtained, which was verified to be zeolite X nanocrystals by XRD, and SEM showed that the zeolite X crys...

Embodiment 3

[0023] Example 3 Zeolite Y nanocrystals were prepared from silica sol, sodium aluminate, sodium hydroxide, 25% tetramethylammonium hydroxide and water. Reaction molar composition: 2.46 (TMA) 2 O: 0.04 Na 2 O: 1Al 2 o 3 : 3.4SiO2 2 :37OH 2O. The reaction process is as follows: first prepare the sodium aluminate sol containing TMA, mix 895g TMA, 5500g water, 6.4g 50% sodium hydroxide solution and 244g sodium aluminate (Al 2 o 3 43%), stirred to make clear precursor solution I. The body-dispelling solution was added to 816g of silica sol (25%), stirred vigorously to obtain a homogeneous solution, and 228.9 grams of glucose was added. Static hydrothermal reaction at 100°C for 2-4 hours, and repeated washing with water to obtain a white final product, which was verified as zeolite Y nanocrystals by XRD, and SEM showed that the zeolite Y crystal grain size was below 80 nanometers.

[0024] Secondly, ethanol is used to disperse the zeolite nanocrystals well, so that it beco...

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Abstract

A multi-class ordered macroporous-microporous material as molecular sieve is prepared from the structure units which is the hydrothermally synthesized nm crystal of micropore molecular sieve (X, Y, A, ZSM-5, beta, TS-1, silicalite-1, etc.) through low-temp. shaping under guide of macroporous template agent and high-temp. demoulding.

Description

technical field [0001] The invention belongs to the field of inorganic porous materials, and in particular relates to a preparation method of a macroporous microporous multilevel ordered pore material. technical background [0002] Microporous materials are widely used in catalysis, separation, adsorption, sensors, etc. However, due to the small void volume of microporous molecular sieves and abundant active hydroxyl groups on the surface, the particles are easily bonded, which makes the mass transfer rate and diffusion rate in the reaction process There are serious defects in the field, which often cause difficulties in material transportation, and the pre-column or membrane pre-pressure is very high. Especially as the use time increases, the particles of microporous molecular sieves bond together, causing more inconvenience in material transportation, not only consumes a lot of energy, but also requires stricter material requirements for equipment, and at the same time inc...

Claims

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Application Information

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IPC IPC(8): C01B39/04
Inventor 赵东元孙锦玉周亚明苗蕾黄立民
Owner FUDAN UNIV