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Method for preparing mesoporous molecular sieve

A technology of mesoporous molecular sieve and active ingredients is applied in the field of preparation of mesoporous molecular sieve MCM-48, which can solve the problems of raw material loss and cost increase, and achieve the effects of reducing preparation cost, reducing usage amount and avoiding toxicity.

Inactive Publication Date: 2013-06-26
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] So far, previous patents such as the patent application No. 201010107602.9 announced on July 14, 2010 and the patent application No. 200510111245.2 announced on May 24, 2006 are all purchased chemical reagents or synthesized silicon sources. Silicon source, which will not only increase the cost but also cause the loss of raw materials during the synthesis process

Method used

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  • Method for preparing mesoporous molecular sieve
  • Method for preparing mesoporous molecular sieve
  • Method for preparing mesoporous molecular sieve

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preparation example Construction

[0022] A preparation method of mesoporous molecular sieve MCM-48, which is characterized in that a single template agent CTAB is used to extract the active ingredients in fly ash as a silicon source, and under the activation of ethanol, it is synthesized by hydrothermal method in an alkaline medium MCM-48, the specific steps are as follows:

[0023] (1) Put the mixture composed of silicon-containing supernatant, template agent CTAB, absolute ethanol and water into the reactor, and stir slowly at 30~40°C until it is completely dissolved. After 2~3 hours of reaction, use H 2 SO 4 The solution adjusted the pH of the mixed solution to be 10.5, and continued to stir for 2 to 3 hours to obtain a white gel;

[0024] (2) Place the obtained white gel in a reaction kettle, control the temperature at 100-110°C, and conduct the crystallization reaction for 60-72 hours. After the reaction, filter and wash, dry to obtain a powdery solid, and roast the sample in a muffle furnace at 500°C A...

Embodiment 1

[0030] Prepare 1000ml of hydrochloric acid solution with a mass fraction of 20%, add 50g of fly ash, stir at a constant speed at 80°C for 4h, filter, wash until neutral, and dry 40g of fly ash for later use. Take 20g of NaOH, prepare 100ml of a solution with a concentration of 5mol / L, add 10g of iron-removing fly ash, stir and reflux at 80°C for 4 hours at normal pressure, then filter to obtain a silicon-containing supernatant (use ICP-AES to measure the silicon content in the supernatant). content), put it aside. According to the molar ratio of silicon-containing supernatant: grinding agent CTAB: absolute ethanol: water = 1:0.5:4.5:100, add reagents, mix and stir, and use 5mol / L H 2 SO 4 The solution adjusts the pH of the mixture to 10.5. Place the obtained white gel in a crystallization kettle, control the temperature at 100°C, and conduct the crystallization reaction for 72 hours, take it out to cool naturally, filter and wash, and dry to obtain a powdery solid. Roast th...

Embodiment 2

[0032] Take 0.05 g of the mesoporous material prepared in Example 1, and add it into 25 mL of an aqueous solution with a lead concentration of 100 mg / L. Finally, a lead removal rate of 95% can be obtained, and a good purification effect has been achieved.

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Abstract

The invention discloses a method for preparing a mesoporous molecular sieve MCM-48. The method comprises the steps of extracting effective ingredients in coal ash as silicon sources by adopting a single template agent cetyl trimethyl ammonium bromide (CTAB); and synthetizing MCM-48 under alkaline medium by a hydrothermal method. The synthetized mesoporous material is regular in ducts, single in aperture distribution, high in order degree, and large in specific surface area. The method is simple and feasible in actual operation, economic and environment-friendly, and can provide a new path for 'recycling' utilization of the coal ash; and the synthetized sample has practical application value.

Description

technical field [0001] The invention relates to a preparation method of a molecular sieve, in particular to a preparation method of a mesoporous molecular sieve MCM-48. Background technique [0002] In 1992, Mobil Corporation of the United States first reported the M41S series of mesoporous molecular sieves. This kind of material has uniform tunable pore size and high specific surface area, and has become a research hotspot in the field of environmental governance. The M41S family of materials includes MCM-41 in the hexagonal phase, MCM-48 in the cubic phase and MCM-50 in the lamellar phase. MCM-48 is more conducive to the diffusion of reactive molecules due to its three-dimensional helical pore structure, higher specific surface area, and higher accessibility. Whether it is used in environmental governance, or in catalysis, nanoclusters Assembly aspects are attractive prospects. [0003] So far, previous patents such as the patent application No. 201010107602.9 announced...

Claims

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Application Information

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IPC IPC(8): C01B39/04B09B3/00
Inventor 孙秀云施筱堃王连军闫惠李健生刘晓东严玉波沈锦优韩卫清黄菲
Owner NANJING UNIV OF SCI & TECH
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