Process of preparing mesoporous molecular sieve with ionic liquid as template agent

A technology of mesoporous molecular sieve and ionic liquid, which is applied in coke cooling, petroleum industry, coke oven, etc., can solve the problem of high crystallization temperature, and achieve the effect of low crystallization temperature and simple preparation process

Inactive Publication Date: 2005-04-27
EAST CHINA NORMAL UNIV
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The synthesis of A1-MCM-41 mesoporous molecular sieves is most commonly found in S under the action of long-chain alkyl trimethyl ammonium (CTMA) cations + I - Supramolecular assembly process (US 6,117,411; US ​​6,712,972; Chem.Mater., 1999, 11:11342), can obtain molecular sieves with higher crystallinity, but the synthesis process requires a higher crystallization temperature of 135-170°C

Method used

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  • Process of preparing mesoporous molecular sieve with ionic liquid as template agent
  • Process of preparing mesoporous molecular sieve with ionic liquid as template agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] The first step template preparation

[0020] Mix N-methylimidazole and hexadecane bromide in a molar ratio of 1:1, react under nitrogen protection at 110°C for 48 hours, cool to room temperature, and obtain a light yellow waxy solid, which is recrystallized with chloroform to obtain a white powder, ionic liquid 1-hexadecyl-3-methylimidazole bromide, namely [C 16 mim]Br;

[0021] Preparation of the second step reaction mixture

[0022] Press Na 2 SiO 3 9H 2 Si in O: [C 16 mim] Br: Al 2 (SO 4 ) 3 Al:H in 2 SO 4 :H 2 The molar ratio of O=1: 0.5: 0.02: 0.8: 124 configure raw materials, prepare reaction mixture (Si / Al=50), under normal temperature, 7.1gNa 2 SiO 3 9H 2 O was dissolved in 12.5 g of deionized water, and 2.67 g of 3.27%wt Al was first added dropwise to the solution 2 (SO 4 ) 3 Aqueous solution, and then add dropwise to the solution containing 4.8g [C 16 mim]Br in water, with H 2 SO 4 Adjust the pH value of the solution to 9.5 to prepare a rea...

Embodiment 2

[0027] Operation process is except following difference, all the other are with embodiment 1:

[0028] Preparation of the second step reaction mixture

[0029] Press Na 2 SiO 3 9H 2 Si in O: [C 16 mim] Br: Al 2 (SO 4 ) 3 Al:H in 2 SO 4 :H 2 The molar ratio of O=1:0.5:0.01:0.8:93 Prepare the raw materials and prepare the reaction mixture (Si / Al=100).

[0030] The third step hydrothermal crystallization

[0031] The raw powder was put into a muffle furnace and calcined at 520°C for 5 hours to obtain Al-MCM-41 mesoporous molecular sieve.

[0032] The XRD spectrum and IR spectrum of the obtained Al-MCM-41 mesoporous molecular sieve are respectively compared with figure 1 and figure 2 similar.

Embodiment 3

[0034] Operation process is except following difference, all the other are with embodiment 1:

[0035] Preparation of the second step reaction mixture

[0036] Press Na 2 SiO 3 9H 2 Si in O: [C 16 mim] Br: Al 2 (SO 4 ) 3 Al:H in 2 SO 4 :H 2 The molar ratio of O=1:0.5:0.05:0.8:106 Prepare the raw materials and prepare the reaction mixture (Si / Al=20).

[0037] The third step hydrothermal crystallization

[0038] The raw powder was put into a muffle furnace and calcined at 580°C for 5h to obtain Al-MCM-41 mesoporous molecular sieve.

[0039] The XRD spectrum and IR spectrum of the obtained Al-MCM-41 mesoporous molecular sieve are respectively compared with figure 1 and figure 2 similar.

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Abstract

The present invention is process of preparing Al-MCM-41 mesoporous molecular sieve with ionic liquid as template agent. The ionic liquid is 1-palmityl-3-methylimidazole bromide, and the material includes sodium silicate, aluminum sulfate, sulfuric acid and water. The preparation process of Al-MCM-41 mesoporous molecular sieve includes the steps of: preparing template agent, preparing the reaction mixture, hydrothermal crystallization, filtering, water washing, drying and roasting. The present invention has the advantages of simple process and low crystallization temperature.

Description

technical field [0001] The invention relates to a method for preparing mesoporous molecular sieves by using ionic liquid as a template, to be precise, relates to a method for preparing Al-MCM-41 mesoporous molecular sieves by using ionic liquid as a template, and belongs to the technical field of inorganic chemical synthesis. Background technique [0002] In 1992, Kresege et al. of Mobil Research and Development Company reported for the first time on Nature, 1992, 359: 710 that the surfactant-long-chain alkyl trimethyl quaternary ammonium salt was used as a template and synthesized under alkaline conditions Mesoporous silicates and aluminosilicates with a single pore size, the structure is long-range order, and the specific surface is 700m 2 / g or more (J. Am. Chem. Soc., 1992, 114: 10834). This material family is called M41S, which includes hexagonal (Hexagonal) MCM-41, cubic (Cubic) MCM-48 and layered structure (Lamellar) MCM-50. Mesoporous m...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C10B39/04
Inventor 杨建国刘彩华于心玉刘月明张欢燕梁学正薛青松何鸣元
Owner EAST CHINA NORMAL UNIV
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