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Prepn process of MCM-48 medium-pore molecular sieve with ternary mixed cationic, non-ionic and anionic surfactant as template agent

A technology of surfactants and mixed cations, which is applied in the field of preparing silicon-based MCM-48 mesoporous molecular sieves, can solve the problems of narrow ingredient range and achieve the effects of simple operation, high regularity and reduced concentration

Inactive Publication Date: 2003-09-10
FUDAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But the range of ingredients is relatively narrow

Method used

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  • Prepn process of MCM-48 medium-pore molecular sieve with ternary mixed cationic, non-ionic and anionic surfactant as template agent
  • Prepn process of MCM-48 medium-pore molecular sieve with ternary mixed cationic, non-ionic and anionic surfactant as template agent
  • Prepn process of MCM-48 medium-pore molecular sieve with ternary mixed cationic, non-ionic and anionic surfactant as template agent

Examples

Experimental program
Comparison scheme
Effect test

example 1 and 2

[0030] Under constant stirring speed, dissolve 0.03mol cetyltrimethylammonium bromide, 0.014mol polyethylene glycol octylphenyl ether and 0.008mol sodium dodecyl carboxylate in appropriate amount of deionized water respectively, mix and stir , then add a certain amount of NaOH solution, after stirring evenly, dropwise add the equivalent of 1mol SiO 2 The silicon source tetraethyl orthosilicate, the mixture was stirred for 1 hour, and then moved into a stainless steel reactor with a polytetrafluoroethylene liner for crystallization at 100°C or 110°C for 4-4.5 days. The product is filtered, washed, and dried at 80°C to obtain the synthetic raw powder. The synthetic raw powder was heated up to 550°C for one hour under nitrogen flow and then fired for 5 hours at 550°C in air to obtain a fired sample. Typical XRD pattern, SEM and TEM photos, N 2 The adsorption-desorption isotherm curve is shown in Figure 1 to Figure 6 .

example 3

[0032] Under constant stirring speed, dissolve 0.024mol polyethylene glycol octylphenyl ether, 0.03mol cetyltrimethylammonium bromide and 0.003mol sodium dodecyl carboxylate in appropriate amount of deionized water respectively, mix and stir , then add a certain amount of NaOH solution, after stirring evenly, dropwise add the equivalent of 1mol SiO 2 The silicon source tetraethyl orthosilicate, the mixture continued to stir for 1 to 1.5 hours, and then moved into a stainless steel reactor with a polytetrafluoroethylene liner and crystallized at 110°C for 4 days. The product is filtered, washed, and dried at 80°C to obtain the synthetic raw powder.

example 4

[0034] Under constant stirring speed, dissolve 0.004mol polyethylene glycol octylphenyl ether, 0.06mol cetyltrimethylammonium bromide and 0.006mol sodium dodecyl carboxylate in appropriate amount of deionized water respectively, mix and stir , then add a certain amount of NaOH solution, after stirring evenly, dropwise add the equivalent of 1mol SiO 2 Silicon source tetraethyl orthosilicate, the mixture was stirred for 1 to 1.5 hours, and then moved into a stainless steel reactor with a polytetrafluoroethylene liner for crystallization at 100°C for 4 days. The product is filtered, washed, and dried at 80°C to obtain the synthetic raw powder.

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Abstract

The present invention prepares high-regularity, high-specific surface area and high-quality silicon-base MCM-48 molecular sieve with ternary mixed water solution of CTAB as cationic surfactant, OP-10 as non-ionic surfactant and SL as anionic surfactant as templating agent, TEOS as silicon source and under very low CTAB / SiO2 molar ratio and very low total surfactant concentration. Into the ternary mixture, alkali source and silicon source are added, and through crystallization, stoving and roasting, the preparation process is completed. The said preparation process has low cost and simple operation, and is environment friendly and suitable for large-scale production.

Description

technical field [0001] The present invention utilizes cetyltrimethylammonium bromide (CTAB, cationic surfactant), polyethylene glycol octylphenyl ether (OP-10, nonionic surfactant) and sodium lauryl carboxylate The ternary mixed aqueous solution of (SL, anionic surfactant) was used as template agent, and tetraethyl orthosilicate (TEOS) was used as silicon source to prepare silicon-based MCM-48 mesoporous molecular sieves. Background technique [0002] MCM-48 is a member of a new type of inorganic porous material M41S series that appeared in the early 1990s. Its Ia3d structure has higher structural symmetry than the p6m structure of MCM-41 with hexagonal phase and one-dimensional pore system. At the same time, MCM-48 has two independent three-dimensional pore systems, which can reduce pore plugging and greatly reduce diffusion restrictions, which is more conducive to the transmission of materials. Therefore, it is used in the application of macromolecular adsorption, separati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B37/02
Inventor 孔令东李全芝
Owner FUDAN UNIV
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