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Method for preparing aluminium-containing MCM-41 molecular sieve

A technology of MCM-41 and molecular sieve, applied in the field of preparation of MCM-41 molecular sieve, can solve problems such as disadvantages, limited application scope, and cost reduction, and achieve high thermal stability and hydrothermal stability, low raw material cost, and hydrothermal stability. Sex-enhancing effect

Inactive Publication Date: 2008-06-25
CHINA UNIV OF PETROLEUM (BEIJING)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method limits the raw material (metakaolin), which limits the scope of application, and does not record the hydrothermal stability characteristics of the prepared mesoporous molecular sieve
[0007] It can be seen that the method for synthesizing MCM-41 molecular sieves using the above-mentioned prior art does not really solve the problem of poor hydrothermal stability of molecular sieves, and the introduction of aluminum sources in most operations is mainly by adding aluminum sulfate, which is not conducive to reducing costs

Method used

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  • Method for preparing aluminium-containing MCM-41 molecular sieve
  • Method for preparing aluminium-containing MCM-41 molecular sieve
  • Method for preparing aluminium-containing MCM-41 molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0025] Dissolve 14.6 grams of CTMAB (content 99%) in 110 milliliters of distilled water, and stir in a water bath at 20°C for 5 hours to form a concentration of 0.13 g / ml of CTMAB solution, then according to the proportion: 100SiO 2 :Al 2 o 3 : 4000H 2 O: 30Na 2 O, while stirring, add water glass (SiO 2 : 5.243 mol / L, Na 2 O: 1.552 mol / L) 38.2 milliliters, and 0.267 grams of pseudo-boehmite (Al 2 o 3 mass content 76.4%), stirred in a water bath at 40°C for 2 hours and mixed evenly to generate a white gel, which was washed with dilute H 2 SO 4 (2 mol / liter) to adjust the pH value to 9-9.5, and the molar composition of the final crystallization reaction system is: 100SiO 2 :20CTMAB:Al 2 o 3 : 4000H 2 O: 30Na 2 O. Continue to stir for 0.5 hours, then transfer to a stainless steel reaction kettle, age at room temperature for 4 hours, crystallize at 120°C for 24 hours, cool to room temperature, filter the product, wash, and dry at 100°C for 12 hours. Roasting at 550° ...

Embodiment 2

[0028] Dissolve 7.3 grams of CTMAB (content 99%) in 55 milliliters of distilled water, and stir in a water bath at 40°C for 0.5 hour to form a concentration of 0.13 g / ml of CTMAB solution, then according to the proportion: 50SiO 2 :Al 2 o 3 : 1000H 2 O: 15Na 2 O, while stirring, add water glass (SiO2 : 5.243 mol / L, Na 2 O: 1.552 mol / L) 38.2 milliliters, and 0.534 grams of pseudo-boehmite (Al 2 o 3 mass content 76.4%). Stir in a water bath at 40°C for 2 hours and mix evenly to form a white gel. 2 SO 4 (2 mol / liter) to adjust the pH value to about 10, and the molar composition of the final crystallization reaction system is: 50SiO 2 :5CTMAB:Al 2 o 3 : 1000H 2 O: 15Na 2 O. Continue to stir for 0.5 hours, then transfer to a stainless steel reactor, age at room temperature for 4 hours, crystallize at 100°C for 72 hours, cool to room temperature, filter the product, wash, and dry at 100°C for 12 hours. Roasting at 550° C. for 6 hours to remove the template agent, obtai...

Embodiment 3

[0031] Dissolve 21.9 grams of CTMAB (content 99%) in 193 milliliters of distilled water, and stir in a water bath at 40°C for 0.5 hour to form a concentration of 0.11 g / ml of CTMAB solution, then according to the proportion: 25SiO 2 : Al 2 o 3 : 1700H 2 O: 30Na 2 O, while stirring, add water glass (SiO 2 : 5.243 mol / L, Na 2 O: 1.552 mol / L) 38.2 milliliters, and 1.068 grams of pseudo-boehmite (Al 2 o 3 mass content 76.4%). Stir in a water bath at 40°C for 2 hours and mix evenly to form a white gel. 2 SO 4 (2 mol / liter) to adjust the pH value to 10.5, the molar composition of the final crystallization reaction system is: 25SiO 2 :7.5CTMAB:Al 2 o 3 : 1700H 2 O: 7.5Na 2 O. Continue to stir for 0.5 hours, then transfer to a stainless steel reaction kettle, age at room temperature for 4 hours, crystallize at 120°C for 48 hours, cool to room temperature, filter the product, wash, and dry at 100°C for 12 hours. Roasting at 550° C. for 6 hours to remove the template agen...

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Abstract

The invention provides a method for preparing an aluminized molecular sieve of MCM-41 (ALMCM-41). The method adopts pseudo-boehmite as aluminum source, sodium silicate as silica source, and cety ltrimethyl ammonium bromide as template. By adopting dilute sulfuric acid to regulate acid, the molecular sieve of ALMCM-41 with high hydrothermal stability is prepared thereby. The invention solves the problem of poor hydrothermal stability of the ALMCM-41 in the prior art. The crystallization retention rate of the molecular sieve of ALMCM-41 prepared in the invention can reach 15 to 50 percent after the ALMCM-41 is aged in 100 percent of steam with temperature of 800 DEG C for 2 hours. The invention can be applied in the industrial preparation of the molecular sieve of ALMCM-41.

Description

technical field [0001] The invention relates to a preparation method of aluminum-containing MCM-41 molecular sieve. Background technique [0002] The mesoporous crystal material was first synthesized by Mobil Corporation. Its pore size can be controlled in the range of 2-10nm, and the pore distribution is uniform. It is named MCM-41. [0003] Pure silicon MCM-41 has only very weak acidity, and its acid strength is only similar to or better than amorphous silicon aluminum, so pure silicon MCM-41 molecular sieve has better thermal stability, but poor hydrothermal stability. Studies have shown that as the silicon on the molecular sieve framework is replaced by aluminum, the acidity also increases. As a mesoporous molecular sieve, MCM-41 has a wide application prospect in hydrocracking due to its large pore size, uniform pore distribution, large specific surface area, strong adsorption capacity, adjustable pore size and acidity, and certain thermal stability. . Therefore, syn...

Claims

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Application Information

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IPC IPC(8): C01B39/04B01J29/04
Inventor 刘百军王辉
Owner CHINA UNIV OF PETROLEUM (BEIJING)
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