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Synthesis method of mesoporous molecular sieve

A technology of mesoporous molecular sieve and synthesis method, applied in the field of synthesis of mesoporous molecular sieve, can solve the problems of increasing synthesis cost, restricting large-scale feeding production and wider application, and no reports, and achieving the effect of reducing synthesis cost.

Inactive Publication Date: 2005-03-16
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the price of chemical reagent raw materials used in the preparation of molecular sieve materials in the above reports is relatively high, especially the use of organic amines such as TEAOH has greatly increased the synthesis cost, limiting its large-scale production and wider application in industry.
Using cheap raw materials such as water glass and aluminum sulfate, the work of "direct method" synthesizing colloidal ZSM-5 zeolite structural unit mesoporous molecular sieves has not been reported so far.

Method used

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  • Synthesis method of mesoporous molecular sieve
  • Synthesis method of mesoporous molecular sieve
  • Synthesis method of mesoporous molecular sieve

Examples

Experimental program
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Effect test

Embodiment 1

[0027] According to the ratio: 4Na 2 O: 80SiO 2 :Al 2 o 3 : 1500H 2 O is sequentially added to water glass (SiO 2 : 3.782 mol / L, Na 2 O: 1.142 mol / L) 158.8 ml, 71.4 ml deionized water, 12.4 ml H 2 SO 4 (6.12 mol / L) and Al with a concentration of (0.8847 mol / L) 2 (SO 4 ) 3 8.48 milliliters of solutions, stirred for 60 minutes and mixed evenly to generate a white gel, then the above-mentioned mixture without high-temperature hydrothermal pretreatment was added to a cetyltrimethylammonium bromide (CTAB) solution with a concentration of 0.06 g / ml , adjust the pH value to about 11 with dilute sulfuric acid, and the molar composition of the final crystallization reaction system is: 80SiO 2 :Al 2 o 3 :4CTAB:2400H 2 O. Stir at room temperature for 30 minutes, then transfer to a stainless steel reactor, crystallize at 100°C for 72 hours, cool to room temperature, filter the product, wash, dry at 80°C for 12 hours, and roast the dried sample at 540°C for 6 hours to remove ...

Embodiment 2

[0030] According to the ratio: 4Na 2 O: 40SiO 2 :Al 2 o 3 : 1000H 2 O is sequentially added to water glass (SiO 2 : 3.782 mol / L, Na 2 O: 1.142 mol / L) 79.4 ml, 47.6 ml deionized water, 6.24 ml H 2 SO 4 (6.12 mol / L) and Al with a concentration of (0.8847 mol / L) 2 (SO 4 ) 3 The solution was 8.48 milliliters, stirred for 60 minutes to mix evenly, and a white gel was formed, and reacted at 140° C. for 32 hours. Then the above-mentioned pretreated mixture is added into a cetyltrimethylammonium bromide (CTAB) solution with a concentration of 0.06 g / ml, and the pH value is adjusted to about 10.5 with dilute sulfuric acid, and the moles of the final crystallization reaction system The composition is: 40SiO 2 :Al 2 o 3 :4CTAB:2400H 2 O. Stir at room temperature for 30 minutes, then transfer to a stainless steel reactor, crystallize at 100°C for 72 hours, cool to room temperature, filter the product, wash, dry at 80°C for 12 hours, and roast the dried sample at 540°C for 6...

Embodiment 3

[0032] The preparation of the colloidal ZSM-5 gel was the same as in Example 2, and the resulting gel was reacted at 140° C. for 46 hours. Then the above-mentioned pretreated mixture is added to the cetyltrimethylammonium bromide (CTAB) solution with a concentration of 0.06 g / ml, and the pH value is adjusted to about 10 with dilute sulfuric acid, and the moles of the final crystallization reaction system The composition is: 40SiO 2 :Al 2 o 3 :4CTAB:2400H 2 O. Stir at room temperature for 30 minutes, then transfer to a stainless steel reactor, crystallize at 100°C for 72 hours, cool to room temperature, filter the product, wash, dry at 80°C for 12 hours, and roast the dried sample at 540°C for 6 hours to remove Template agent to obtain the said mesoporous molecular sieve of the present invention. Its XRD pattern is as follows image 3 .

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Abstract

The invention discloses a synthesis method of mesoporous molecular sieve by using soluble silicate and aluminium sulphate for synthesizing mesoporous molecular screen containing ZSM-5 zeolite preliminary structural unit, wherein a direct method is employed to obtain nano zeolite particles containing zeolite preliminary structural unit, then self-assembling is conducted to cationic surface active agent hexadecyl trimethyl-ammonium bromide to obtain the MCM-41 molecular sieve.

Description

Technical field: [0001] The invention relates to a method for synthesizing mesoporous molecular sieves, which is a method for synthesizing mesoporous molecular sieves containing ZSM-5 zeolite primary structural units by using direct method colloidal ZSM-5 as a precursor. Background technique: [0002] Since the scientists of Mobil Corporation (J.Am.Chem.Soc., 114, 10834, 1992) successfully synthesized mesoporous molecular sieves in 1992, due to the material's regular and adjustable pore size, high BET surface area and pore volume, and high thermal stability It has become a hot spot in the research of catalytic materials. Especially in heavy oil processing and organic chemical reactions involving macromolecules, it should have broad application prospects. However, because the pore walls of mesoporous molecular sieves are in an amorphous state, compared with microporous zeolite crystals, mesoporous molecular sieves have lower hydrothermal stability and acidity, which greatly ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/38C01B39/46
Inventor 肖强项寿鹤
Owner NANKAI UNIV
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