Method for pressure hydrothermal synthesis of MCM-41 mesoporous molecular sieve

A medium-porous molecular sieve, MCM-41 technology, applied in the direction of crystalline aluminosilicate zeolite, etc., can solve problems such as the inability to meet the requirements of catalytic process structural stability, achieve easy operation, improved thermal and hydrothermal stability, synthesis simple method effect

Inactive Publication Date: 2003-03-12
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Description
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  • Application Information

AI Technical Summary

Problems solved by technology

Although this method improves the stability of MCM-41 to a certain extent, it still cannot meet the requirements of catalytic technology for structural stability.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The raw material is TEOS:H 2 O: CTACl: NaOH = 1.0: 130: 0.4: 0.4 molar ratio mixed and stirred evenly, then transferred to a polytetrafluoroethylene-lined autoclave, filled with 10.0MPa nitrogen, and then crystallized at 120 ° C for 48h, the The obtained product was filtered, washed with water and dried, and calcined at 550°C for 6 hours to remove the template agent, and then the molecular sieve was subjected to heat and hydrothermal treatment. The intensity retention rate of the XRD100 diffraction peak after treatment is shown in Table 1.

Embodiment 2

[0018] Press the raw material by Na 2 SiO 3 :H 2 O:CTAB:NH 3 ·H 2 The ratio of O=1.0:175:0.5:0.15 was mixed and then transferred to an autoclave, filled with 8MPa nitrogen, crystallized at 140°C for 35h, filtered, washed and dried, and then calcined at 650°C for 4h to remove the template agent. The data of molecular sieve after thermal and hydrothermal treatment are shown in Table 1.

Embodiment 3

[0020] The raw material is TEOS:H 2 O:CTAOH:NH 3 ·H 2 The ratio of O=1.0:40:0.08:0.25 was mixed and then transferred to the autoclave and filled with 14.5MPa nitrogen gas. After crystallization at 80°C for 72h, the product was filtered, washed and dried, and roasted at 500°C for 10h to remove the template agent, and then the molecular sieve After thermal and hydrothermal treatment, the results are shown in Table 1.

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Abstract

A process for synthesizing the mesoporous molecular sieve MCM-41 includes mixing template agent with water and alkali catalyst, adding Si source, stirring to obtain mother liquid, feeding it in high-pressure reactor with teflon liner, filling nitrogen gas, heating, crystallizing, cooling, filtering, water washing, drying, heating, and calcining to remove template agent. The product has high stability.

Description

[0001] Field: [0002] The invention belongs to a synthesis method of MCM-41 mesoporous molecular sieves, in particular to a pressurized hydrothermal synthesis method of MCM-41 mesoporous molecular sieves with high heat and high hydrothermal stability. Background technique [0003] In 1992, the Mobil Petroleum Company of the United States first launched the M41S series of new mesoporous SiO 2 Materials (C T Kresge, M E Leonowicz, W J Roth, J C Vartuli and J S Beck, Nature, 1992, 359, 710.), among which MCM-41 mesoporous molecular sieves are the most attractive. Because of its narrow pore size distribution, large specific surface area and strong adsorption capacity, MCM-41 has broad application prospects and academic research value in the fields of catalysis, ion exchange, adsorption separation and advanced inorganic materials. However, the poor thermal and hydrothermal stability of MCM-41 is the main limiting factor in its practical application. (Gao Xionghou, Mao Xuewen, et...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/04
Inventor 孙予罕张晔吴东彭少逸
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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