Method for directly synthesizing Al-MCM-41 mesoporous molecular sieve from kaolin or Hangjin 2# soil

A technology of mesoporous molecular sieve and kaolin, applied in the direction of crystalline aluminosilicate zeolite, nanotechnology, etc., to achieve the effect of reducing process energy consumption, saving synthesis cost and shortening synthesis time

Active Publication Date: 2017-05-31
INNER MONGOLIA NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The method overcomes existing technical defects by accurately controlling conditions such as template concentration, synthesis temperature, and synthesis pH value.

Method used

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  • Method for directly synthesizing Al-MCM-41 mesoporous molecular sieve from kaolin or Hangjin 2# soil

Examples

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Embodiment 1

[0016] Synthesis of Al-MCM-41 mesoporous molecular sieve from coal-series kaolin 1: Mix coal-series kaolin 1 and 4mol / L sulfuric acid at a ratio of 1g:10mL, boil and reflux for 2 hours, cool naturally, wash with water once to neutral, suction filter, 60 ℃ drying for 6 hours to obtain acidified kaolin 1. Take 100 mL of 0.2 mol / L sodium hydroxide aqueous solution and keep the temperature in a water bath at 70°C; add 1.5 g of CTABr and stir to dissolve it; then add 4 g of acidified kaolin 1 and continue stirring for 1 hour; add 1 mol / L sulfuric acid dropwise to adjust the pH of the solution =10, continue stirring for 1 hour. The obtained mixture was transferred into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and was allowed to stand at 110° C. for 12 hours for crystallization. After natural cooling, the obtained product was suction-filtered and washed with water once until neutral; the solid product was dried at 60°C for 6 hours, and then calcined in an air at...

Embodiment 2

[0018] Synthesis of Al-MCM-41 mesoporous molecular sieve from coal-series kaolin 2: Mix coal-series kaolin 2 and 4mol / L sulfuric acid at a ratio of 1g:10mL, boil and reflux for 2 hours, cool naturally, wash with water once to neutral, suction filter, 60 ℃ drying for 6 hours to obtain acidified kaolin 2. Take 100 mL of 0.2 mol / L sodium hydroxide aqueous solution and keep the temperature in a water bath at 70°C; add 1.5 g of CTABr and stir to dissolve it; then add 4 g of acidified kaolin 2 and continue stirring for 1 hour; add 1 mol / L sulfuric acid dropwise to adjust the pH of the solution =10, continue stirring for 1 hour. The obtained mixture was transferred into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and was allowed to stand at 110° C. for 12 hours for crystallization. After natural cooling, the obtained product was suction-filtered and washed with water once until neutral; the solid product was dried at 60°C for 6 hours, and then calcined in an air at...

Embodiment 3

[0020] by Hang Jin 2 # Synthesis of Al-MCM-41 Mesoporous Molecular Sieves from Earth: Hang Jin 2 # Soil and 4mol / L sulfuric acid were mixed at a ratio of 1g:10mL, boiled and refluxed for 2 hours, cooled naturally, washed with water once until neutral, filtered with suction, dried at 60°C for 6 hours to obtain acidified Hangjin 2 # Soil (activated clay). Take 100 mL of 0.2 mol / L sodium hydroxide aqueous solution and keep the temperature in a water bath at 70°C; add 1.5 g of CTABr and stir to dissolve it; then add 4 g of activated clay and continue stirring for 1 hour; add 1 mol / L sulfuric acid dropwise to adjust the pH of the solution. 10. Continue stirring for 1 hour. The obtained mixture was transferred into a polytetrafluoroethylene-lined hydrothermal reaction kettle, and was allowed to stand at 110° C. for 12 hours for crystallization. After natural cooling, the obtained product was suction-filtered and washed with water once until neutral; the solid product was dried at...

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Abstract

The invention relates to a method for directly synthesizing Al-MCM-41 mesoporous molecular sieve from kaolin or Hangjin 2# soil. The method comprises (1) carrying out acid activation on layered clay raw ore through a sulfuric acid aqueous solution having a concentration of 4 mol / L to obtain acidified clay, (2) mixing the acidified clay and a hexadecyl trimethyl ammonium bromide alkaline solution having a certain concentration in a water bath at a temperature of 70 DEG C for 1h, adjusting pH to 10 and carrying out stirring for 1h, (3) putting the mixture into a hydrothermal reactor and carrying out standing crystallization at a temperature of 110 DEG C for 12h, and (4) washing the product through water and carrying out drying and calcination to obtain an Al-MCM-41 mesoporous molecular sieve. The method is free of high energy consumption pretreatment processes such as high temperature calcination, high speed ball milling or high temperature alkali melting, greatly reduces the use amount of a template agent, produces the by-product of aluminum sulfate octadecahydrate, is simple and reduces a cost.

Description

technical field [0001] The present invention relates to a kind of low energy consumption made of kaolin or Hangjin 2 # A method for directly synthesizing Al-MCM-41 mesoporous molecular sieves from layered clay minerals such as soil belongs to the field of inorganic non-metallic materials. Background technique [0002] In 1992, Mobil R&D personnel used structural self-assembly technology and used cetyltrimethylammonium bromide (CTABr) as a template to synthesize MCM-41 mesoporous cells with uniform channels and hexagonal orderly arrangement for the first time. Molecular sieves (Nature, 1992, 359, 710-712). The era of ordered mesoporous molecular sieves has come. MCM-41 mesoporous molecular sieve has attracted the attention of researchers because of its wide application in the fields of catalysis, adsorption, separation and purification. There are endless reports on the synthesis of MCM-41 mesoporous molecular sieves using organic or inorganic silicon reagents as raw materi...

Claims

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Application Information

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IPC IPC(8): C01B39/04B82Y40/00
CPCB82Y40/00C01B39/04C01P2002/30C01P2004/64C01P2006/12C01P2006/14C01P2006/16
Inventor 王奖徐爱菊李冰贾美林照日格图
Owner INNER MONGOLIA NORMAL UNIVERSITY
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