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Preparation method and application of meso-porous material loaded with metal tin through chemical vapor deposition

A technology of chemical vapor deposition and mesoporous materials, applied in chemical instruments and methods, organic chemistry, chemical recycling, etc., can solve problems such as safety hazards, complex catalyst preparation process, and long cycle, so as to avoid the damage of oxidants and improve the selectivity sex, cheap effect

Inactive Publication Date: 2016-10-12
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the preparation process of the catalyst is complicated and the cycle is long, and the silica gel needs to be treated with concentrated nitric acid at high temperature, so there are certain safety hazards

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] 5g amorphous SiO 2 The carrier was placed in a muffle furnace and raised to 400°C at a rate of 5°C / min, kept for 5h for calcination, cooled to room temperature and taken out. The fired amorphous SiO 2 The carrier is placed in a corundum tube, put the corundum tube into a tube furnace, and activate it at 400°C for 2 hours under the protection of nitrogen, with a space velocity of 10 minutes -1 . Rapidly raise the temperature to 540°C, and after the temperature stabilizes, pass SnCl 4 / N 2 Airflow 1.5h. Stop feeding SnCl 4 / N 2 , switch to N 2 , the flow rate increased to 200mL / min, and roasted in a nitrogen atmosphere at 540°C for 5h. Stop the heating of the tube furnace and keep N 2 Continuous feeding to purge the unreacted SnCl on the surface of the catalyst 4 and HCl, and the tail gas was absorbed with absolute ethanol. After naturally cooling down to room temperature, the solid catalyst was taken out and recorded as Sn / SiO 2 .

[0039] The following exam...

Embodiment 2

[0043] Take 0.30 g of the catalyst prepared in Example 1, 2.94 g of cyclohexanone and 15 mL (about 11.8 g) of acetonitrile, and add them into a 50 mL three-necked flask. Heat up to 70°C while stirring, and after the temperature stabilizes, add 5.10 g of 30% H 2 o 2 Solution, constant temperature reaction 24h. After cooling to room temperature, the reaction solution was taken out for analysis. The conversion of cyclohexanone was 41%, and the selectivity of caprolactone was 96%.

Embodiment 3

[0045] 5g of MCM-41 carrier was taken to load metal tin according to the operation steps of Example 1, and the prepared catalyst was designated as Sn / MCM-41. According to the operation process of embodiment 2, the difference from embodiment 2 is that the selected catalyst for the reaction is Sn / MCM-41. The conversion of cyclohexanone was 43%, and the selectivity of caprolactone was 92%.

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Abstract

The invention discloses a preparation method of a meso-porous material loaded with metal tin through chemical vapor deposition, and an application of the meso-porous material in the Baeyer-Villiger oxidation reaction of cyclohexanone. A tin-containing compound and a meso-porous material undergo a gas-solid reaction in oxygen-free environment to make the metal element tin be loaded on the meso-porous material, and when the meso-porous material loaded with metal tin is used to catalyze the Baeyer-Villiger oxidation reaction of cyclohexanone, the highest conversion rate is greater than 50%, and the highest cyclohexanone selectivity can exceed 95%. Compared with other catalysts containing metal active components, the catalyst disclosed in the invention has the advantages of simple preparation process and high load capacity. When the meso-porous material loaded with metal tin is used in the Baeyer-Villiger oxidation reaction of cyclohexanone with hydrogen peroxide or alkyl peroxide as an oxygen source, reaction conditions are mild, the catalyst is easy to recycle, and use of organic peroxoic acid is avoided, thereby the potential safety hazard and the environment pollution are eliminated.

Description

technical field [0001] The invention relates to the technical field of fine chemicals, in particular to a preparation method of a mesoporous material loaded with metal tin by chemical vapor deposition and its application in the Baeyer-Villiger oxidation reaction of cyclohexanone. Background technique [0002] ε-caprolactone is an important organic synthesis intermediate and polymer monomer, mainly used in the production of synthetic rubber, synthetic resin and synthetic fiber, and can also be used in the synthesis of polycaprolactone, caprolactam, caprolactone, adipic di Raw materials for acids, adhesives and elastomers, etc. In addition, ε-caprolactone can also be used as a raw material for high-performance fibers and the preparation of medical materials due to its large tensile elongation, good air permeability, and unique biocompatibility and degradability. The traditional Baeyer-Villiger oxidation reaction of cyclohexanone is generally a peroxyacid, such as trifluoroper...

Claims

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Application Information

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IPC IPC(8): B01J23/14C07D313/04B01J29/03B01J29/04
CPCY02P20/584B01J23/14B01J29/0308B01J29/041B01J2229/183C07D313/04
Inventor 吴剑邓渊婷马桃桃管凡凡
Owner XIANGTAN UNIV
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