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Method for synthesizing ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve by using hard template

A synthesis method and multi-level pore technology, applied in the direction of crystalline aluminosilicate zeolite, can solve problems such as limitations, and achieve the effects of improving catalytic activity, improving flow and diffusion performance, and shortening material transport paths

Active Publication Date: 2014-09-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the controllable synthesis of hierarchical pore order of hierarchical zeolite molecular sieves is limited to the order of mesopores or macropores, and there is no hierarchical zeolite molecular sieve with ordered macropores and ordered mesopores. to report

Method used

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  • Method for synthesizing ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve by using hard template
  • Method for synthesizing ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve by using hard template
  • Method for synthesizing ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve by using hard template

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] Example 1 Dissolve 1.52g of 1M aqueous solution of tetrapropylammonium hydroxide in 23.84g of deionized water, then add 0.69g of tetraethylorthosilicate dropwise into the above solution, and stir at 20°C for 24h to obtain a uniform Mixed solution; add 0.75g 10wt% titanium isopropoxide / isopropanol mixed solution to the obtained mixed solution, stir at 20°C for 8h to obtain a precursor solution; add 0.3g ordered macroporous-mesoporous hierarchical The carbon material (macropore diameter is 400nm, mesopore diameter is 20nm) is immersed in 20g of the prepared precursor solution and mixed evenly, the obtained mixture is moved to a 100mL hydrothermal reaction kettle, and hydrothermally heated at 130°C for 12h; the obtained product Wash and filter with deionized water for 5 times, then immerse in the newly prepared precursor solution again, carry out the second hydrothermal reaction under the same conditions, and repeat this 6 times; the final obtained TS-1 molecular sieve nanocr...

Embodiment 2

[0039] Dissolve 1.52g of 1M tetrapropylammonium hydroxide aqueous solution in 23.84g of deionized water, stir evenly, then add 0.69g of tetraethyl orthosilicate dropwise into the above solution, and stir at 20°C for 24h to obtain a uniform 0.10g15wt% titanium isopropoxide / isopropanol mixed solution was added to the mixed solution obtained, and stirred at 20°C for 8h to obtain a precursor solution; 0.4g ordered macroporous-mesoporous multi-level The porous carbon material (with a macropore diameter of 400nm and a mesopore diameter of 20nm) was immersed in 25g of the precursor solution prepared above and mixed evenly, and the obtained mixture was transferred to a 100mL hydrothermal reaction kettle, and hydrothermally heated at 100°C for 12h; The obtained product was washed with deionized water for 5 times and then immersed in the newly prepared precursor solution again, and the second hydrothermal reaction was carried out under the same conditions, and this was repeated 8 times; ...

Embodiment 3

[0042] Dissolve 1.52g of 1M tetrapropylammonium hydroxide aqueous solution in 23.84g of deionized water, stir evenly, then add 0.69g of tetraethyl orthosilicate dropwise into the above solution, and stir at 40°C for 8h to obtain a uniform 2.4g 5wt% titanium isopropoxide / isopropanol mixed solution was added to the mixed solution obtained, and stirred at 40°C for 2h to obtain a precursor solution; 0.2g ordered macroporous-mesoporous multi-level The porous carbon material (with a macropore diameter of 400nm and a mesopore diameter of 30nm) was immersed in 15g of the prepared precursor solution and mixed evenly, and the obtained mixture was transferred to a 50mL hydrothermal reactor, and heated at 110°C for 12h; the obtained The product was washed with deionized water and filtered for 5 times, then immersed in the newly prepared precursor solution again, and the second hydrothermal reaction was carried out under the same conditions, and this was repeated 7 times; the final TS-1 mol...

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Abstract

The invention discloses a method for synthesizing an ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve TS-1 by using a hard template. The method comprises the following steps: with a three-dimensional ordered macroporous-mesoporous hierarchical carbon material as a hard template, performing limited-range growth of TS-1 nanocrystals in a three-dimensional ordered cage type mesoporous canal of the hard template by adjusting and controlling hydrothermal synthesis conditions according to a hydrothermal synthesis method of the TS-1 nanocrystals, and removing the hard template to obtain the ordered macroporous-mesoporous-microporous hierarchical-pore molecular sieve TS-1. The method disclosed by the invention is simple and feasible, synthetic conditions are easy to control, and the cycle is short; the molecular sieve TS-1 prepared by adopting the method has a novel ordered macroporous-mesoporous-microporous hierarchical pore structure, mesopores are uniform and controllable in diameter, and the method has an important promotion effect on expansion of application of the molecular sieve TS-1 in the field of catalysis.

Description

technical field [0001] The invention relates to the technical field of molecular sieve synthesis, in particular to a method for preparing and regulating the molecular sieve macropore-mesopore-micropore ordered channel structure. Background technique [0002] Epoxy compounds are important intermediates in organic synthesis, widely used in petrochemical, fine chemical and organic synthesis industries, and play a pivotal role in the national economy. Titanium-silicon molecular sieve catalyst TS-1 is an important catalyst for epoxidation reaction. It selectively catalyzes the epoxidation reaction of olefins by selecting low-concentration hydrogen peroxide as the oxidant, and the by-product is water. Titanium-silicon molecular sieve catalyst TS-1 has no pollution in the catalytic oxidation process, and the reaction conditions are mild, which overcomes the shortcomings of serious pollution and lengthy reaction process in the traditional process. However, the size of its micropore...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/08C01B39/04
Inventor 陈丽华孙明慧李昱邓兆苏宝连
Owner WUHAN UNIV OF TECH
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