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Method for encapsulating homogeneous catalyst in pore channels of mesoporous molecular sieve

A homogeneous catalyst and mesoporous molecular sieve technology, applied in molecular sieve catalysts, chemical instruments and methods, catalyst activation/preparation, etc., can solve problems such as difficult separation and non-reusable use, achieve low price, realize separation and repeated use , the effect of a wide range of raw material sources

Active Publication Date: 2017-12-29
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In order to solve the problem that most existing metal complexes are difficult to separate and cannot be reused as homogeneous catalysts, the purpose of the present invention is to provide a packaged homogeneous catalyst that realizes easy separation of homogeneous catalysts and can be reused. Catalyst in the channel of mesoporous molecular sieve

Method used

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  • Method for encapsulating homogeneous catalyst in pore channels of mesoporous molecular sieve
  • Method for encapsulating homogeneous catalyst in pore channels of mesoporous molecular sieve
  • Method for encapsulating homogeneous catalyst in pore channels of mesoporous molecular sieve

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0042] Dissolve b in dichloromethane with magnetic stirring to make a 0.001 g / mL solution. According to the ratio of molecular sieve volume and vacuum chamber as 1:10, put SBA-15 into a vacuum bottle to pump air, and pump SBA-15 at 120°C for 12 hours, and then press the mass ratio of b to SBA-15 1:0.01, inject the prepared homogeneous solution into the vacuum bottle containing SBA-15 and stir vigorously for 12 hours, then drain the dichloromethane solvent in the system at 40°C in vacuum, and the obtained sample is b / SBA-15 15.

[0043] Weigh sample b / SBA-15 and place it on a quartz plate, and smear it evenly with petroleum ether to control the thickness at 1 mm. Then place the dried quartz sheet in vacuum atomic layer deposition (ALD) equipment. Deposition of Al on SBA-15 orifices by atomic layer deposition 2 o 3 Implement encapsulation. The set deposition parameters are as follows: the deposition temperature is 100° C., the temperature of the reaction source trimethylalu...

Embodiment 2

[0046] Dissolve c in toluene and stir magnetically to form a 0.01g / mL solution. According to the ratio of molecular sieve volume and vacuum chamber as 1:50, put MCM-41 into a vacuum bottle to pump air. At 80°C, pump MCM-41 for 24 hours, and then press c and the mass of MCM-41 The ratio is 1:10, inject the prepared homogeneous solution into the vacuum bottle containing MCM-41 and stir vigorously for 18 hours, then drain the toluene solvent in the system at 60°C in vacuum, and the obtained sample is c / MCM-41 .

[0047] Weigh the sample c / MCM-41 and place it on a quartz plate, and smear it evenly with ethanol to control the thickness at 2 mm. Then place the dried quartz sheet in vacuum atomic layer deposition (ALD) equipment. Deposition of TiO at MCM-41 Orifices by Atomic Layer Deposition 2 Implement encapsulation. The deposition parameters are set as follows: the deposition temperature is 60° C., the temperatures of the reaction source titanium tetraisopropoxide and water ar...

Embodiment 3

[0050] Dissolve d in chloroform with magnetic stirring to make a 1 g / mL solution. According to the ratio of molecular sieve volume to vacuum chamber 1:100, put SBA-16 into a vacuum bottle to pump air, and pump SBA-16 at 100°C for 18 hours, and then press the mass ratio of d to SBA-16 1:100, inject the prepared homogeneous solution into the vacuum bottle containing SBA-16 and stir vigorously for 24 hours, then drain the chloroform solvent in the system at 80°C in vacuum, and the obtained sample is d / SBA-16.

[0051] Weigh sample d / SBA-16 and place it on a quartz plate, and smear it evenly with dichloromethane to control the thickness at 0.5 mm. Then place the dried quartz sheet in vacuum atomic layer deposition (ALD) equipment. Encapsulation is achieved by depositing ZnO at the orifice of SBA-16 by atomic layer deposition. The deposition parameters are set as follows: the deposition temperature is 50° C., the temperatures of the reaction source diethyl zinc and water are 60° ...

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Abstract

A method for encapsulating a homogeneous catalyst in pore channels of a mesoporous molecular sieve comprises the following steps: the mesoporous molecular sieve is fed into a vacuum container, air is extracted, a well prepared homogeneous catalyst solution is injected into the vacuum container containing the molecular sieve, a sample is obtained after stirring and vacuumizing, placed on a quartz plate and smeared uniformly with a diluting agent, the aired quartz plate is placed in a low-temperature vacuum atomic layer deposition equipment, an oxide precursor is subjected to primary pulse treatment and air-suppressing reaction, and a physically absorbed part is removed through air extraction; secondary pulse treatment is performed, steam and the oxide precursor are subjected to the air-suppressing reaction, and unreacted materials are discharged through air extraction; the two steps are repeated, an oxide is obtained through deposition on the surface of a sample base, the total thickness of a film is controlled by changing the cycling times of the two steps, and the size of pores, at seals, of the mesoporous molecular sieve is controlled. The method has the advantage that the homogeneous catalyst is easy to separate and is recyclable.

Description

technical field [0001] The invention belongs to a catalyst and a preparation method, in particular to a method for encapsulating a homogeneous catalyst in a channel of a mesoporous molecular sieve. Background technique [0002] Metal complex catalysts, especially homogeneous catalysts with chiral ligands, are very important for the development of chemical, biological and pharmaceutical industries. However, these homogeneous catalysts often have the problems of difficult recovery and product separation, causing their application to bring environmental and product quality problems. At present, the immobilization of homogeneous catalysts to obtain heterogeneous catalysts is an important way to achieve effective separation after the reaction. Compared with traditional covalently bonded heterogeneous catalysts, nanoreactors are constructed by non-covalently encapsulating homogeneous catalysts into mesoporous or mesoporous molecular sieve channels, showing a degree of freedom com...

Claims

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Application Information

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IPC IPC(8): B01J31/22B01J31/24B01J29/03B01J37/02B01J37/10
CPCB01J29/0341B01J31/2217B01J31/2495B01J37/0205B01J37/0221B01J37/0244B01J37/10B01J2531/842B01J2531/845B01J2531/46B01J2531/56B01J2531/821B01J2531/0266B01J2531/0252B01J2229/186B01J35/23
Inventor 覃勇张斌张淑芳梁浩杰谷晓敏葛会宾
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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