Preparation method of mesoporous zeolite molecular sieve

A mesoporous zeolite and molecular sieve technology, applied in the direction of crystalline aluminosilicate zeolite, borocarbane silicone crystalline aluminum silicate zeolite, etc., to achieve high catalytic activity

Inactive Publication Date: 2013-12-18
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

If anionic polymers are used, no electrostatic interaction will occur, so there have been no reports in the literature of introducing anionic polymers into molecular sieve synthesis systems to form mesopores

Method used

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  • Preparation method of mesoporous zeolite molecular sieve
  • Preparation method of mesoporous zeolite molecular sieve
  • Preparation method of mesoporous zeolite molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Example 1: Synthesis of mesoporous silicalite-1 using a polyelectrolyte-surfactant complex as a template

[0020] Synthetic raw materials: polyacrylic acid (PAA), cetyltrimethylammonium bromide (CTAB), tetrapropylammonium hydroxide (TPAOH), tetraethylorthosilicate (TEOS), sodium chloride (NaCl), ten Octyldimethyl[trimethoxysilylpropyl]ammonium chloride (TPOAc).

[0021] Synthetic ratio: 10SiO 2 : 3.6TPAOH: 0.08TPOAc: 360H 2 O: 4.2NaCl

[0022] Synthesis steps: a certain amount of NaCl was dissolved in 5 ml of deionized water, and 25% TPAOH was added to form a clear solution. Add this solution to the previously synthesized CTAB and PAA complex, and stir for 20 minutes. TEOS and a small amount of TPOAc (50% in methanol) were added to the solution with stirring. Finally, stir at room temperature for 2 h to obtain a uniform mixed emulsion. Put it in a reaction kettle, and crystallize it with water at 140°C for 6 days. The obtained product was suction filtered, washed...

Embodiment 2

[0027] Example 2: Adding NaCl to synthesize mesoporous silicalite-1

[0028] Synthetic raw materials: polyacrylic acid (PAA), cetyltrimethylammonium bromide (CTAB), tetrapropylammonium hydroxide (TPAOH), tetraethylorthosilicate (TEOS), sodium chloride (NaCl), ten Octyldimethyl[trimethoxysilylpropyl]ammonium chloride (TPOAc).

[0029] Synthesis steps: directly add 25% TPAOH to the compound of CTAB and PAA, stir for 20min, the solution is still milky white. TEOS and a small amount of TPOAc (50% methanol solution) were added to the solution with stirring, and stirred for 30 min. Finally, dissolve a certain amount of NaCl in 5ml of water and add it to the above solution. Stir mechanically at room temperature for 2 h to obtain a viscous emulsion. Put it in a reaction kettle, and crystallize it with water at 140°C for 6 days. The obtained product was suction filtered, washed, dried at 80°C, and calcined at 550°C for 6h.

[0030] Mesoporous silicalite-1 was synthesized by using ...

Embodiment 3

[0033] Example 3: Synthesis of mesoporous silicalite-1 using other polyelectrolyte-surfactant complexes as templates

[0034] Synthetic raw materials: polyacrylic acid (PAA), cetylpyridinium chloride (CPC), tetrapropylammonium hydroxide (TPAOH), tetraethylorthosilicate (TEOS), sodium chloride (NaCl), octadecyl Dimethyl[trimethoxysilylpropyl]ammonium chloride (TPOAc).

[0035] Synthesis steps: the same as the steps of mesoporous silicalite-1 in Example 1, except that the cationic surfactant is changed into cetylpyridinium chloride (CPC).

[0036] The final effect of the mesoporous silicalite-1 synthesized by this method is not much different from the characterization in Example 1.

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Abstract

The invention provides a preparation method of mesoporous zeolite by utilizing a polyelectrolyte-surfactant composite as a template, and belongs to the technical field of organic chemistry, physical chemistry, and catalytic chemistry. The preparation method comprises following steps: utilizing conventional silicon source and aluminum source, taking a low cost anion polyelectrolyte-surfactant composite as a template, adopting an one-pot method, hydrothermally crystallizing at the temperature of 140 DEG C, and burning at the temperature of 550 DEG C for 6 hours so as to obtain mesoporous silicalite-1 and mesoporous ZSM-5. The preparation method utilizes the polyelectrolyte (polyacrylic acid PAA)-surfactant (cetyl trimethyl ammonium bromide CTAB) composite as the template to prepare mesoporous zeolite with hole sizes of 5 to 20 nm, mesoporous ZSM-5 has a high catalytic activity in catalytic reactions; the adding sequence of NaCl is changed so as to synthesize mesoporous silicalite-1 with a hole size of about 3 nm, furthermore, the mesopores are smaller and the array of mesopores is tighter; mesoporous silicalite-1 can also be prepared from another polyelectrolyte (polyacrylic acid PAA)-surfactant (cetyl pyridinium chloride) composite, indicating that the method of synthesizing mesoporous zeolite by utilizing a polyelectrolyte-surfactant composite as the template can be widely popularized, and has a potential application value in the field of catalysis.

Description

technical field [0001] The invention belongs to inorganic chemistry, physical chemistry, material chemistry and catalytic chemistry, and in particular relates to the preparation technology of mesoporous zeolite synthesized by template method. Background technique [0002] Zeolite materials are widely used in the fields of catalysis, adsorption and ion exchange because of their good hydrothermal stability, strong acidity and shape selectivity [see Corma A.Chem.Rev., 1997, 97, 2373-2419.] . However, the micropores of zeolite molecular sieves are very small (generally less than 1 nanometer), which is not conducive to the diffusion of reactants. In order to solve this problem, mesoporous materials with regular channels and high specific surface area represented by MCM-41 came into being [Kresge C T, Leonowicz M E, Roth W J. Nature, 1992, 359, 710-712.]. However, due to the weak hydrothermal stability and low acidity of such mesoporous materials, they cannot be widely used in t...

Claims

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Application Information

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IPC IPC(8): C01B39/04C01B39/40
Inventor 陈铁红刘金玉王金桂
Owner NANKAI UNIV
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