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Method for preparing mesoporous molecular sieve by sepiolite

A mesoporous molecular sieve and sepiolite technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve the problems of restricting the industrial production and application of mesoporous materials, expensive raw materials, complicated methods, etc., and achieve solid acidity enhancement and high diffusion capacity , good shape selectivity

Inactive Publication Date: 2005-09-21
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0002] The preparation of mesoporous molecular sieve materials is usually based on the synthesis of pure silicon mesoporous materials from organosilicon, and then the skeleton is replaced to obtain doped mesoporous molecular sieves. These methods are complicated and the raw materials are expensive. Environmental pollution restricts the large-scale industrial production and application of mesoporous materials

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] After the sepiolite is treated with 2M hydrochloric acid for 12 hours, the sepiolite with low magnesium content is obtained, and its composition is: SiO 2 64.5%, CaO 0.26%, MgO 1.7%, H 2 O 33.2%;

[0020] Dissolve NaOH in distilled water to obtain a pH 12 solution, add CTAB and tetramethylammonium bromide, CTAB:SiO 2 0.1~0.5:1, CTAB:Tetramethylammonium bromide is 1:1~5; the treated sepiolite is added to the solution, the solid-liquid ratio is 15:100, and the dispersion is vigorously stirred for 1 hour to obtain a suspension;

[0021] Pour the suspension into a high-pressure reactor, raise the temperature to 120°C, react at a pressure of 15 atm for 36 hours, then reduce the pressure and cool, and then wash with water under vacuum to obtain a white solid;

[0022] The white solid was burned at a temperature of 823K for 8 hours to obtain a white mesoporous molecular sieve material;

[0023] The XRD pattern of the mesoporous molecular sieve material is shown in Figure 1...

Embodiment 2

[0025] After the sepiolite is treated with 2M hydrochloric acid for 12 hours, the sepiolite with low magnesium content is obtained, and its composition is: SiO 2 64.5%, CaO 0.26%, MgO 1.7%, H 2 O 33.2%;

[0026] NaOH was dissolved in distilled water to obtain a solution of pH 12, and the content of CTAB and tetramethylammonium bromide was added, CTAB:SiO 2 0.5~1.2:1, CTAB:tetramethylammonium bromide is 1:0.2~0.8;

[0027] Add treated sepiolite to the solution, the solid-to-liquid ratio is 15:100, and disperse with strong stirring for 1 hour to obtain a suspension;

[0028] Pour the suspension into a high-pressure reactor, raise the temperature to 120°C, react at a pressure of 15 atm for 36 hours, then reduce the pressure and cool, and then wash with water under vacuum to obtain a white solid;

[0029] The white solid was burned at a temperature of 823K for 8 hours to obtain a white mesoporous molecular sieve material;

[0030] After crystallization, the mesoporous molecul...

Embodiment 3

[0032] After the sepiolite is treated with 2M hydrochloric acid for 12 hours, the sepiolite with low magnesium content is obtained, and its composition is: SiO 2 64.5%, CaO 0.26%, MgO 1.7%, H 2 O 33.2%;

[0033] Add NaAlO to the suspension at pH 12 2 Stir for 1 hour, pour the suspension into a high-pressure reactor, raise the temperature to 120°C, react at a pressure of 15 atm for 36 hours, then reduce the pressure and cool, then cool, vacuum, filter and wash with water to obtain a white solid;

[0034] The white solid was burned at a temperature of 723K for 8 hours to obtain a white mesoporous molecular sieve material;

[0035] The XRD pattern of the mesoporous molecular sieve material is shown in Figure 3, which shows that it is an ALHMS mesoporous molecular sieve with a specific surface area of ​​570m 2 / g, the average pore diameter is 4.2nm.

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Abstract

The invention relates to the method for preparing mesoporous molecular sieve by sepiolite which consists of fragmenting sepiolite, treating with 2M-6M hydrochloric acid, sulfuric acid or nitric acid for 8-16h, removing magnesium compounds and obtaining non-shaped silicon dioxide, then subjecting aluminium salts and surface active agent to water thermal crystallization in water solution, filtering with crystallized sepiolite, washing with deionized water or extracting with organic solvent to obtain molecular sieve precursor, then burning the precursor for 3-18h in Muffle furnace at the temperature of 300-600 deg. C.

Description

Technical field: [0001] The invention relates to the field of inorganic non-metallic materials, and uses natural layered silicate or aluminosilicate as raw material to prepare mesoporous molecular sieves, especially hydrothermal sepiolite with a pore diameter of 3-5 nm and a specific surface area greater than 700m 2 / g of hexagonal molecular sieve (HMS), aluminum-containing hexagonal molecular sieve (ALHMS), highly structured mesoporous silica (SBA), aluminum-containing highly structured mesoporous silica (ALSBA) mesoporous molecular sieves for petroleum cracking catalysts , fine organic synthesis catalysts, adsorbents, microelectronics, etc. Background technique: [0002] The preparation of mesoporous molecular sieve materials is usually based on the synthesis of pure silicon mesoporous materials from organosilicon, and then the skeleton is replaced to obtain doped mesoporous molecular sieves. These methods are complicated and the raw materials are expensive. Environmenta...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/02
Inventor 金胜明杨华明邱冠周宋晓岚
Owner CENT SOUTH UNIV
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