Proess for preparing mesoporous molecular sieve MCM-48 by using mixture of cationic surfactant and non-ionic surfactant as template agent

A non-ionic surface, mixed cation technology, applied in the field of MCM-48 mesoporous molecular sieve, can solve the problems of pollution, poor hydrothermal stability, cumbersome and other problems, and achieve uniform pore size distribution, improved hydrothermal stability, and easy operation.

Inactive Publication Date: 2003-01-15
FUDAN UNIV
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  • Abstract
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Problems solved by technology

But the neutral amine in this synthetic route pollutes the environment
Ryoo et al. used mixed cationic surfactant CTAB and nonionic surfactant C 12 (EO) 3 Synthesized MCM-48 with better hydrothermal stability, but the synthesis process needs to adjust the pH several times or add salts, so it is cumbersome, and the silicon source needs to be prepared by yourself
The above work has greatly improved the synthesis of MCM-48, but its disadvantages of poor hydrothermal stability have not been significantly improved, and the use of cheap silicon sources is also a practical need

Method used

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  • Proess for preparing mesoporous molecular sieve MCM-48 by using mixture of cationic surfactant and non-ionic surfactant as template agent
  • Proess for preparing mesoporous molecular sieve MCM-48 by using mixture of cationic surfactant and non-ionic surfactant as template agent
  • Proess for preparing mesoporous molecular sieve MCM-48 by using mixture of cationic surfactant and non-ionic surfactant as template agent

Examples

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example 1

[0022] At a constant stirring speed, add a certain amount of water glass dropwise into the 4:1 mixed aqueous solution of CTAB and OP-10, and stir at 30°C for 1 hour to obtain a molar composition of 1.0 SiO 2 :0.15CTAB:0.03OP-10:0.282Na 2 O: 58H 2 O mixture. Move the mixture into a stainless steel reaction kettle and let it stand at 100°C for 2 days. The product is washed, filtered and then dried to obtain the synthetic MCM-48. The sample was directly calcined at 650°C in air for 5 hours, and then heated to 850°C for 2 hours to obtain MCM-48 mesoporous molecular sieve. Typical XRD pattern, TEM photo, N 2 Adsorption-desorption isotherms and thermal analysis results are shown in Figure 1 to Figure 4 . And the XRD figure, N of the sample after thermal and hydrothermal treatment 2 Adsorption-desorption isotherms and pore structure parameters are shown in Figure 5 , Figure 6 and table one. Table.1 Pore structure parameters of MCM-48 sample Sample Unitcell BET Pore Pore F...

example 2

[0029] The process of preparing synthetic MCM-48 is the same as Example 1. Take the synthetic MCM-48 and directly roast it in the air at 650°C for 5 hours to obtain the MCM-48 mesoporous molecular sieve

example 3

[0031] At 20°C, add a certain amount of water glass dropwise into a 10:1 mixed aqueous solution of CTAB and OP-10 and stir for 1 hour to obtain a molar composition of 1.0 SiO 2 :0.30CTAB:0.02OP-10:0.282Na 2 O: 58H 2 O mixture. The mixture was transferred into a stainless steel reaction kettle, crystallized at 100°C for 3 days, the product was washed, filtered and then dried to obtain synthetic MCM-48. The sample was first calcined at 550°C in nitrogen for 1 hour, and then calcined at 700°C for 4 hours to obtain MCM-48 mesoporous molecular sieve.

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Abstract

An MCM-48 mesoporous molecular sieve is prepared from industrial water glass as Si source and the template agent which is the mixture of cationic surfactant CTAB and non-ionic surfactant OP-10. Its advantages are high high-temp and hydrothermal stability, low cost and less pollution.

Description

technical field [0001] The present invention utilizes cetyltrimethylammonium bromide (CTAB, cationic surfactant) and polyethylene glycol octyl phenyl ether (OP-10, nonionic surfactant) mixed aqueous solution as template agent, with industrial Using grade water glass as the silicon source, a high-heat, hydrothermally stable MCM-48 mesoporous molecular sieve was prepared. Background technique [0002] M41s series mesoporous molecular sieves are a new class of inorganic porous materials that appeared in the early 1990s, including three mesoporous molecular sieves: MCM-41 in hexagonal phase, MCM-48 in cubic phase and MCM-50 in lamellar phase. Among them, MCM-50 in the lamellar phase is thermally unstable, MCM-41 in the hexagonal phase is easy to synthesize, and MCM-48 in the cubic phase has a complex structure and harsh synthesis conditions. However, because the Ia3d structure of MCM-48 has higher structural symmetry than the p6m structure of MCM-41, and its two independent thr...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 李全芝赵伟孔令东王利军
Owner FUDAN UNIV
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