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A kind of preparation method and application of nano-Cu elemental modified sba-15

A cu-pc, 1. cu-pc technology, applied in the direction of sulfide preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of nanoscale difference, easy collapse of frame structure, easy oxidation, etc. , to achieve high hydrothermal stability, improve reaction efficiency, and not easy to oxidize

Active Publication Date: 2022-07-15
CHINA THREE GORGES UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, when the framework structure of MOFs participates in the reaction, if the reaction conditions are a little harsh, the framework structure will easily collapse and cannot be recycled and utilized again. Therefore, the stability of the framework of MOFs as a catalyst has not been effectively solved. The field has also been extensively studied by many researchers
[0003] In order to solve the problem that MOFs are very easy to collapse as a catalyst framework, previous people thought of directly retaining the active component part and directly calcining it to prepare it into a carbon (C)-supported active component catalyst. However, such operations, calcination The organic part is carbonized, and the remaining metal active components are exposed to the air, which is easily oxidized, and most of the calcined metal particles are micron-sized, which is far from the nano-sized
After carbonization, during the reaction, affected by the solvent and stirring force, the metal active components are easy to fall off. Although it can be recycled and reused for the second time, the catalytic activity will be greatly reduced.

Method used

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  • A kind of preparation method and application of nano-Cu elemental modified sba-15
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  • A kind of preparation method and application of nano-Cu elemental modified sba-15

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Effect test

Embodiment 2

[0040] A preparation method of SBA-15 modified by nano-Cu elemental substance - the number of revolutions is 1600r / min, and the crystallization is carried out at 160°C for 20h. The following are the specific embodiments:

[0041] Weigh 1.0 g of copper nitrate trihydrate (Cu(NO) 3 ) 2 ·3H 2 O) and 0.90 g trimesic acid (H 3 BTC) was added to 60 mL of deionized aqueous solution and stirred continuously until Cu(NO 3 ) 2 ·3H 2 O and H 3 BTC was completely dissolved; 1.6g of tetramethylammonium hydroxide (TMA) was then weighed into the dissolved system, the revolution of the stirrer was set to 1600r / min, and vigorously stirred for 20min; 1.0g of the prepared rod-shaped SBA-15 medium was weighed pore molecular sieve, slowly stirred into the mixed solution, and stirred continuously for 25 minutes at room temperature; the mixed solution after stirring was transferred to a crystallization kettle lined with polytetrafluoroethylene, and continued to be crystallized at a high temper...

Embodiment 3

[0045] A nano-scale Cu-based material catalytic synthesis - 5-chloro-2-(phenylthio)phenol, the following is the specific embodiment (catalyst dosage 19.78wt%):

[0046] Weigh 0.2313 g (1.6 mmol) of compound 4-chlorothiophenol 1a on an analytical balance into a round-bottomed flask, use a Pasteur dropper to measure 4 mL of dimethyl sulfoxide (DMSO) as a solvent, and then weigh Cs 2 CO 3 0.65g (2mmol) was used as a base, 19.78wt% of the Cu-PC@SBA-15 catalyst prepared in Example 2 was added, and finally 0.0816g (0.4mmol) of the compound iodobenzene 2a was added, and the reaction was carried out under constant temperature stirring at 120°C. , and then refluxed; TCL monitored the reaction, after 2h, the compound iodobenzene 2a reacted completely, the system was cooled to room temperature, the solvent DMSO was extracted and evaporated, and the reaction system was separated by column chromatography on a silica gel column to obtain the target product 3a; Combined (GC-MS) detection a...

Embodiment 4

[0050] A nano-scale Cu-based material catalytic synthesis - 5-chloro-2-(phenylthio)phenol, the following is the specific embodiment (catalyst dosage 9.89wt%):

[0051] Weigh 0.2313 g (1.6 mmol) of compound 4-chlorothiophenol 1a on an analytical balance into a round-bottomed flask, use a Pasteur dropper to measure 4 mL of dimethyl sulfoxide (DMSO) as a solvent, and then weigh Cs 2 CO 3 0.65g (2mmol) was used as a base, and 9.89wt% of the Cu-PC@SBA-15 catalyst prepared in Example 2 was added. Finally, 0.0816g (0.4mmol) of the compound iodobenzene 2a was added, and the reaction was carried out under constant temperature stirring at 120°C. , and then refluxed; TCL monitored the reaction, after 2h, the compound iodobenzene 2a reacted completely, the system was cooled to room temperature, the solvent DMSO was extracted and evaporated, and the reaction system was separated by column chromatography on a silica gel column to obtain the target product 3a; The yield of the target produ...

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Abstract

The invention relates to a preparation method and application of nano-Cu element-modified SBA-15; the rod-shaped SBA-15 mesoporous molecular sieve is used as a load support, MOFs is used as a copper source, and H 2 O is the synthesis solvent. The metal-organic framework MOFs were loaded with the unique two-dimensional hexagonal channels of the mesoporous molecular sieve SBA-15, and then the target product Cu-PC@SBA-15 with in-situ generation of nano-Cu was prepared by different calcination methods and calcination temperatures. The catalyst Cu-PC@SBA-15 prepared by the invention does not use other solvents in the loading process, is green and environmentally friendly, has low cost and simple process for catalyst preparation, and participates in the catalytic C-H activation reaction with a yield of up to 92%, and more reused.

Description

technical field [0001] A preparation method and application of nano-Cu element-modified SBA-15. Background technique [0002] Mesoporous molecular sieve SBA-15 is a silicon-based material with a unique two-dimensional hexagonal structure. Its unique pore channels not only have large pore volume and uniform pore diameter distribution, but also enjoy high specific surface area and thick pore walls. SBA-15 is used as a base to wrap other materials with catalytic properties into new catalysts. During catalysis, the reaction time is shorter, the catalytic yield is higher, and it can be separated and reused for many times. It has received many researches in this field. widespread attention of scholars. Organometallic framework MOFs, which are microporous materials, are not only used in gas storage, but also in the field of catalysis. However, when the framework structure of MOFs participates in the reaction, if the reaction conditions are slightly harsh, the framework structure ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J29/03C07C319/14C07C323/20
CPCB01J29/0333C07C319/14B01J2229/186C07C323/20
Inventor 王龙罗享豪孙宏媛胡为民李东升
Owner CHINA THREE GORGES UNIV