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Preparation method and catalytic application of organic-inorganic hybrid ZOF-TS-1 molecular sieve

A technology of ZOF-TS-1 and molecular sieve, which is applied in molecular sieve catalysts, organic compound/hydride/coordination complex catalysts, organic chemistry, etc., and can solve problems such as different hydrolysis rates and inhomogeneous molecular sieve precursor solutions

Active Publication Date: 2021-09-24
WUHAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the hydrolysis rate of different organosilicon sources is different, which easily leads to the inhomogeneity of the molecular sieve precursor solution

Method used

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  • Preparation method and catalytic application of organic-inorganic hybrid ZOF-TS-1 molecular sieve
  • Preparation method and catalytic application of organic-inorganic hybrid ZOF-TS-1 molecular sieve
  • Preparation method and catalytic application of organic-inorganic hybrid ZOF-TS-1 molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] A preparation method of organic-inorganic hybrid ZOF-TS-1 molecular sieve, the specific steps are as follows:

[0037] (1) Dissolve 1.70g (0.005mol) of analytically pure bis(triethoxysilyl)methane (BTESM) in 5.08g of tetrapropylammonium hydroxide (TPAOH) aqueous solution (TPAOH is 0.005mol, and the concentration of the aqueous solution is 1mol / L, the mass percentage is 20wt%), and stirred at room temperature for 4h until BTESM is completely hydrolyzed to obtain a clear solution;

[0038] (2) Dissolve 18.75g (0.09mol) analytically pure tetraethyl silicate (TEOS) in 45.76g tetrapropylammonium hydroxide aqueous solution (TPAOH is 0.045mol, aqueous solution concentration is 1mol / L, mass percent is 20wt%) , stirred at room temperature for 4 hours, until TEOS was completely hydrolyzed to obtain a clear and transparent solution;

[0039] (3) Mix the solutions obtained in (1) and (2) evenly, and stir at room temperature for 30 minutes;

[0040] (4) 1.70 g of analytically pur...

Embodiment 2

[0046] A preparation method of organic-inorganic hybrid ZOF-TS-1 molecular sieve, the specific steps are as follows:

[0047] (1) Dissolve 3.41g (0.01mol) of analytically pure bis(triethoxysilyl)methane (BTESM) in 10.17g of tetrapropylammonium hydroxide (TPAOH) aqueous solution (TPAOH is 0.01mol, and the concentration of the aqueous solution is 1mol / L, the mass percentage is 20wt%), and stirred at room temperature for 4h until BTESM is completely hydrolyzed to obtain a clear solution;

[0048] (2) Dissolve 16.67g (0.08mol) of analytically pure tetraethyl silicate (TEOS) in 40.67g of tetrapropylammonium hydroxide aqueous solution (TPAOH is 0.04mol, the aqueous solution concentration is 1mol / L, and the mass percentage is 20wt%) , stirred at room temperature for 4 hours, until TEOS was completely hydrolyzed to obtain a clear and transparent solution;

[0049] (3) Mix the solutions obtained in (1) and (2) evenly, and stir at room temperature for 30 minutes;

[0050] (4) 1.70 g ...

Embodiment 3

[0056] A preparation method of organic-inorganic hybrid ZOF-TS-1 molecular sieve, the specific steps are as follows:

[0057] (1) Dissolve 8.51g (0.025mol) of analytically pure bis(triethoxysilyl)methane (BTESM) in 25.42g of tetrapropylammonium hydroxide (TPAOH) aqueous solution (TPAOH is 0.025mol, and the concentration of the aqueous solution is 1mol / L, the mass percentage is 20wt%), and stirred at room temperature for 4h until BTESM is completely hydrolyzed to obtain a clear solution;

[0058] (2) 10.42g (0.05mol) analytically pure tetraethyl silicate (TEOS) was dissolved in 25.42g tetrapropylammonium hydroxide aqueous solution (TPAOH is 0.025mol, aqueous solution concentration is 1mol / L, mass percent is 20wt%) , stirred at room temperature for 4 hours, until TEOS was completely hydrolyzed to obtain a clear and transparent solution;

[0059] (3) Mix the solutions obtained in (1) and (2) evenly, and stir at room temperature for 30 minutes;

[0060] (4) 1.70 g (0.005 mol) o...

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Abstract

The invention relates to a preparation method of an organic-inorganic hybrid ZOF-TS-1 molecular sieve, which comprises the following steps: respectively dissolving bis (triethoxysilyl) methane and tetraethyl silicate in an aqueous solution of tetrapropylammonium hydroxide for hydrolysis to obtain hydrolysate A and hydrolysate B; uniformly mixing the hydrolysate A and the hydrolysate B, adding tetrabutyl titanate, uniformly mixing, adding a hydrogen peroxide solution and deionized water, and uniformly mixing to obtain a precursor solution; and carrying out pre-crystallization treatment on the precursor solution, then carrying out hydrothermal crystallization treatment, and roasting the obtained solid product to obtain the organic-inorganic hybrid ZOF-TS-1 molecular sieve. Compared with a traditional synthesis method, a pre-hydrolysis technology is adopted, the problem that the hydrolysis rates of bis (triethoxysilyl) methane and tetraethyl silicate are inconsistent is solved, a pre-crystallization technology is beneficial to the nucleation crystallization process of the molecular sieve, a methylene structure can be embedded into a molecular sieve framework to obtain the high-crystallinity molecular sieve, when the catalyst is applied to epoxidation reaction of chloropropene, a more excellent catalytic effect is achieved.

Description

technical field [0001] The invention belongs to the technical field of catalytic materials, and in particular relates to a preparation method and catalytic application of an organic-inorganic hybrid TS-1 molecular sieve. Background technique [0002] TS-1 (titanium silicalite-1) type titanium-silicon molecular sieve is a kind of molecular sieve material formed by replacing some Si atoms in MFI molecular sieve with heteroatom Ti. Because the Ti species in the framework of TS-1 molecular sieve has catalytic epoxidation activity, hydrogen peroxide is used as the oxidant, and the by-product is water, which can achieve excellent catalytic activity under mild conditions, so TS-1 is regarded as a A green and efficient epoxidation catalyst is often used in the epoxidation of olefins, alkanes, alcohols and aromatic compounds to produce important chemical raw materials. [0003] However, the epoxidation reaction catalyzed by the TS-1 molecular sieve material is a heterogeneous reacti...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J29/89B01J31/38C01B39/06C07D301/12C07D303/08
CPCB01J29/89B01J31/38C01B39/065C07D301/12C07D303/08C01P2002/86C01P2004/32
Inventor 陈丽华余申李小云李昱阳晓宇苏宝连
Owner WUHAN UNIV OF TECH
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