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Process for preparing shape-controllable big-pore mesoporous molecular sieve

A technology of mesoporous molecular sieve and large pore size, which is applied in the direction of crystalline aluminosilicate zeolite, etc., and can solve the problems of limited application

Inactive Publication Date: 2002-07-03
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the application-related forming research, that is, the research on the shape control of the ultra-large pore mesoporous material SBA-15 is still blank, which greatly limits its application.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Example 1. Dissolve 40g of P123 (Aldrich, EO20PO70EO20, average molecular weight of 5800) in 300g of water, add 1200g of hydrochloric acid solution (2mol / Kg), stir at 35℃ to make a clear and transparent solution, and then add four orthosilicate 85 g of ethyl ester, stirred and reacted at 35°C for 20 hours to obtain a white precipitate, which was transferred to a polytetrafluoroethylene container and hydrothermally reacted at 80°C statically for 24-72 hours. Observed under an optical microscope, the white product was wheat ear-like. The yield is 98%

[0028] The transmission electron micrograph shows the SBA-15 structure in a hexagonal arrangement. The pore diameter is about 80, and the specific surface area is as high as 800m 2 / g, the pore volume is 1.4cm 3 / g. The thermal stability is higher than 850°C.

Embodiment 2

[0029] Example 2: Dissolve 20g of P123 in 450g of water, add 300g of hydrochloric acid solution (4mol / Kg), stir at 35~40℃ to make a clear and transparent solution, then add 31g of tetramethyl orthosilicate at 40℃ The reaction was stirred and reacted for 20 hours to obtain a white gel solution, which was transferred to a polytetrafluoroethylene container and hydrothermally reacted at 100°C for 24 hours. Observed under an optical microscope, the fiber is a silica fiber with colorful spots. The yield was 80%.

[0030] The main physical indicators of mesoporous molecular sieve fibers: the interface diameter is 10 microns, and the length is 5-6 mm. From the scanning electron microscope, it is composed of a beam of about 300nm. The transmission electron micrograph shows the SBA-15 structure in a hexagonal arrangement, in which the channels are parallel to the main axis of the fiber. The pore diameter is around 90, and the specific surface area is as high as 800m 2 / g, the pore volume i...

Embodiment 3

[0031] In Example 3, 20g of P123 was dissolved in 300g of water and 150g of DMF, followed by adding 300g of hydrochloric acid solution (4mol / Kg), stirring at 35~40℃ to make a clear and transparent solution, followed by 44g of tetraethyl orthosilicate, The reaction was stirred at 40°C for 20 hours to obtain a gel solution, which was transferred to a polytetrafluoroethylene container, and hydrothermally reacted at 80°C for 24-72 hours. Observed under a scanning electron microscope, the white product was doughnut-shaped. The yield is 100%

[0032] The transmission electron micrograph of the mesoporous molecular sieve shows a hexagonal SBA-15 structure with a pore size of about 94  and a specific surface area of ​​up to 800 m 2 / g, the pore volume is 1.4cm 3 / g. The thermal stability is higher than 850°C.

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PUM

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Abstract

A process for synthesizing the form-controllable big-pore mesoporous molecular sieve SBA-15 features that the non-ionic surfactant P123 is used as structure guiding agent, and such methods are used as changing Si source, adding auxiliary solvent, electrolyte and surfactant, and using static, ultrasonic and microwaev interface growth method. Its advantages are different forms (sphere, fibre, ring, etc) and wide application range.

Description

Technical field [0001] The invention belongs to the technical field of molecular sieve inorganic materials, and specifically relates to a method for synthesizing large-pore mesoporous molecular sieves with controllable morphology (pore size greater than 40 ), and mainly refers to a method for synthesizing SBA-15 with large pores and different morphologies. . technical background [0002] In 1992, researchers from the US Mobil Company first reported on Nature the M41S series of mesoporous molecular sieves with high specific area and high degree of order. People have conducted extensive research on synthesis and its applications in catalysis and adsorption. Complete statistics. Since 1997, there have been hundreds of patent documents in this area. Mainly related to the preparation of mesoporous molecular sieves and some application issues, including applications such as catalysis, adsorption and separation, sensors, microelectrodes, electron microscopy probes, light guides and som...

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屠波
Owner FUDAN UNIV
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