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Nano-crystallite and non-ionic surface active agent microwave self-assembling preparation method for mesopore and micropore molecular sieve

A non-ionic surface, microporous molecular sieve technology, applied in the field of preparation of medium-micro double-porous molecular sieves, can solve the problems of limited practical application of mesoporous molecular sieves, insufficient catalytic activity, poor hydrothermal stability, etc., and achieve reasonable distribution and uniform nucleation. , the effect of short crystallization time

Inactive Publication Date: 2011-01-19
SOUTH CHINA UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But in practice, mesoporous molecular sieves have their fatal weaknesses: their properties are similar to amorphous aluminosilicates, their acidity is weak, their hydrothermal stability is poor, and their catalytic activity is not enough.
This greatly limits the practical application of mesoporous molecular sieves

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] (1) Preparation of microporous molecular sieve nanocrystals: add 10ml of deionized water into a clean and dry conical flask, stir at 200 rpm and add 0.025mol of tetraethylammonium hydroxide and 0.0016mol of isopropanol For aluminum, 0.075 mol of ethyl orthosilicate was slowly added dropwise, and then stirred at a speed of 300 rpm for 2 hours to adjust the pH to 11. Put the reaction solution into a polytetrafluoroethylene reactor, set the MARS-5 microwave workstation power to 300W, the heating rate to 20°C / min, and to crystallize at 100°C for 1 hour.

[0028] (2) Self-assembly of nanocrystals and non-ionic surfactants: Dissolve 0.03mol polyoxyethylene lauryl ether in 16.5ml deionized water, and slowly add dropwise to the microporous molecular sieve nanocrystals obtained in (1) In the crystal, stirring was continued at a speed of 200 rpm for 2 hours to adjust the pH to 8. Put the reaction solution into a polytetrafluoroethylene reactor, set the MARS-5 microwave workstation ...

Embodiment 2

[0031] (1) Preparation of microporous molecular sieve nanocrystals: add 12ml of deionized water into a clean and dry conical flask, stir at 250 rpm and add 0.01mol of tetramethylammonium hydroxide (TMAOH) and 0.001mol Sodium aluminate, slowly add 0.05 mol ethyl orthosilicate dropwise, stir at 400 rpm for 2 hours, adjust the pH to 11. The reaction solution was put into a polytetrafluoroethylene reactor, the MARS-5 microwave workstation power was set to 90W, the heating rate was 10°C / min, and the crystallization was performed at 140°C for 90 minutes.

[0032] (2) Self-assembly of nanocrystals and nonionic surfactants: Dissolve 0.005mol of polyoxyethylene myristyl ether in 16.5ml of deionized water, and slowly add dropwise to the microporous molecular sieve nanocrystals obtained in (1) In the crystal, stir at 300 rpm for 2 hours to adjust the pH to 5. Put the reaction solution into a polytetrafluoroethylene reactor, set the MARS-5 microwave workstation power to 300W, heating rate a...

Embodiment 3

[0035] (1) Preparation of microporous molecular sieve nanocrystals: Add 15ml of deionized water into a clean and dry Erlenmeyer flask, stir at 300 rpm and add 0.03mol of tetrabutylammonium chloride (TBAC) and 0.005mol Aluminum isopropoxide, 0.2 mol methyl orthosilicate was slowly added dropwise, and stirred at a speed of 500 rpm for 5 hours, and the pH was adjusted to 12. The reaction solution was put into a polytetrafluoroethylene reactor, the MARS-5 microwave workstation power was set to 480W, the heating rate was 40°C / min, and the crystallization was performed at 160°C for 105 minutes.

[0036] (2) Self-assembly of nanocrystals and nonionic surfactants: Dissolve 0.05mol polyoxyethylene stearyl ether in 20ml of deionized water, and slowly add dropwise to the microporous molecular sieve nanocrystals obtained in (1) In the process, stirring was carried out at 400 rpm for 4 hours, and the pH was adjusted to 10. Put the reaction solution into a polytetrafluoroethylene reactor, set...

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Abstract

The invention discloses a preparation method of medium and micro sized diplopore molecular sieve by microwave auto-assmebly of nano microcrystal and nonionic surfactant, which comprises the steps that: deionized water is added into a cone-shaped bottle and then microporous template agent and aluminum source agent are added and stirred for 2 -5 hours, and then the pH value is adjusted; the reaction liquid is put into a reactionary pot to be crystallized for 1 to 3 hours, so as to obtain the microporous molecular sieve nanometer microcrystal; the nonionic surfactant is dissolved into the deionized water and is dripped into the obtained microporous molecular sieve nanometer microcrystal to be stirred, and then the pH value is adjusted; the reaction liquid is sent into polytetrafluoroethylenereaction pitcher to be crystallized for 0.5 to 2 hours; the obtained material is washed, dried, baked and demouded, and the medium and micro sized diplopore molecular sieve is finally made. By using different template agent and nonionic surfactant, the invention realizes bimodal pore structure of material and control of pore diameter, thus enhancing acidity of mesopore material and hydrothermal stability, ensuring nucleation of the nano micro crystal to be more uniform and the crystallized time to be shorter with high repeatability.

Description

Technical field [0001] The invention relates to a method for preparing a medium-micro double-hole molecular sieve, in particular to a method for preparing a medium-micro double-hole molecular sieve by microwave self-assembly of nano crystals and a nonionic surfactant. Background technique [0002] Microporous molecular sieve has a well-developed microporous structure and strong acidity. It is an important selective catalyst in the modern petroleum industry. However, due to the small pore size, it is difficult for large-diameter molecules to enter the pores on the one hand, and large molecules formed in the pores. Can not escape quickly, often lead to side reactions, and greatly reduce its application range. With the development of the modern chemical industry and the heavyization of petroleum, the catalytic cracking of heavy oil and residual oil has become the controlling factor of the petroleum catalytic cracking process. At the same time, due to the needs of coal chemical and b...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B39/04C01B37/00
Inventor 奚红霞陈汇勇郑东东李忠
Owner SOUTH CHINA UNIV OF TECH
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