Iridium-based bipyridine-organosilicon nanotube heterogeneous catalyst and preparation method

A technology based on bipyridine and organosilicon, which is applied in the field of iridium-based bipyridine-organosilicon nanotube heterogeneous molecular catalysts and its preparation, can solve the problems of poor stability of homogeneous molecular catalysts, difficulty in recycling, and restrictions on industrial applications, and achieve easy Recovery can be recycled, good stability, low requirements for equipment and equipment

Inactive Publication Date: 2019-09-17
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] However, due to the shortcomings of homogeneous molecular catalysts such as poor stability and difficulty in recovery after reaction, their industrial application is greatly limited.

Method used

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  • Iridium-based bipyridine-organosilicon nanotube heterogeneous catalyst and preparation method
  • Iridium-based bipyridine-organosilicon nanotube heterogeneous catalyst and preparation method
  • Iridium-based bipyridine-organosilicon nanotube heterogeneous catalyst and preparation method

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Step 1: Add 2.952g of diisopropylamine and 80mL of tetrahydrofuran into a 250mL beaker at -10°C under anhydrous nitrogen atmosphere, then add 1.74g of n-butyllithium dropwise and stir well. Afterwards, 1.21g of 4,4'-dimethyl-2,2'-bipyridine was added dropwise and stirred, and then 2.62g of 3-chloropropyltrimethoxysilane was slowly added and stirred for 12h, and the above mixture was reacted overnight Then add acetone to quench, finally evaporate the solvent, and obtain 4,4'-[4-(trimethoxysilane)butyl]-2,2'-bipyridine after vacuum drying. Synthesis process see figure 1 .

[0033] Step 2: Mix 0.875g KCl and 0.275g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO 20 -PO 70 -EO 20 (P123) was dissolved in 120mL 2M hydrochloric acid solution, stirred rapidly to form a uniform transparent solution, added 3.15mmol organosilane precursor 1,4‐bis(triethoxysilyl)benzene and continued to stir vigorously, reducing the stirring rate Continue to s...

Embodiment 2

[0038] Step 1: Add 1.476g of diisopropylamine and 80mL of tetrahydrofuran into a 250mL beaker at -5°C under anhydrous nitrogen atmosphere, then add 0.87g of n-butyllithium dropwise and stir well. Afterwards, 1.21g of 4,4'-dimethyl-2,2'-bipyridine was added dropwise and stirred, and then 3.93g of 3-chloropropyltrimethoxysilane was slowly added and stirred for 18h, and the above mixture was reacted overnight Then add acetone to quench, finally evaporate the solvent, and obtain 4,4'-[4-(trimethoxysilane)butyl]-2,2'-bipyridine after vacuum drying. Synthesis process see figure 1 .

[0039] Step 2: Mix 1.75g ​​KCl and 0.55g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO 20 -PO 70 -EO 20 (P123) was dissolved in 120mL of 1.8M hydrochloric acid solution, stirred rapidly to form a uniform and transparent solution, added 2.8mmol organosilane precursor 1,4-bis(triethoxysilyl)benzene and continued to stir vigorously, reduce the stirring Continue stir...

Embodiment 3

[0044] Step 1: Add 0.738g of diisopropylamine and 80mL of tetrahydrofuran into a 250mL beaker at 0°C under anhydrous nitrogen atmosphere, then add 0.435g of n-butyllithium dropwise and stir well. After that, 1.21g of 4,4'-dimethyl-2,2'-bipyridine was added dropwise and stirred, and then 5.24g of 3-chloropropyltrimethoxysilane was slowly added and stirred for 24h, and the above mixture was reacted overnight Then add acetone to quench, finally evaporate the solvent, and obtain 4,4'-[4-(trimethoxysilane)butyl]-2,2'-bipyridine after vacuum drying. Synthesis process see figure 1 .

[0045] Step 2: Mix 3.5KCl and 1.1g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO 20 -PO 70 -EO 20 (P123) was dissolved in 120mL 2.2M hydrochloric acid solution, stirred rapidly to form a uniform transparent solution, added 2.45mmol organosilane precursor 1,4-bis(triethoxysilyl)benzene and continued to stir vigorously, reduce the stirring Continue stirring at a hi...

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Abstract

The invention relates to an iridium based dipyridine-organic silicon nanotube heterogeneous catalyst and a preparation method thereof. A composite of 4,4'-[4-(trimethoxysilane)butyl]-2,2'-dipyridine coordinated dichloro(pentamethylcyclopentadienyl) iridium dimer is filled into an organic silicon nanotube. Potassium chloride, a template, a organic silane precursor 1,4-di(triethoxysilyl)benzene, and 4,4'-[4-(trimethoxysilane)butyl]-2,2'-dipyridine are added into a hydrochloric acid solution in sequence to obtain a mixture; the mixture is added into a mixed solution of ethanol and hydrochloric acid to obtain a solid product namely dipyridine-organic silicon nanotube, and finally the dipyridine-organic silicon nanotube and dichloro(pentamethylcyclopentadienyl) iridium dimer carry out reactions to obtain the iridium based dipyridine-organic silicon nanotube heterogeneous catalyst. The catalyst has a clear channel structure and large specific surface area. A novel feasible method is provided for the immobilization of homogeneous molecular catalysts.

Description

technical field [0001] The invention relates to a brand-new iridium-based bipyridine-organosilicon nanotube heterogeneous molecular catalyst and a preparation method thereof, belonging to the synthesis and application of organosilicon composite materials. Background technique [0002] Mesoporous nanotubes refer to one-dimensional porous nanomaterials with pore diameters ranging from 2 to 50 nm and regular pore distribution. Due to its high specific surface area and strong mechanical and thermal stability, it is widely used in the fields of heterogeneous catalysis, gas adsorption, and electronic devices. Existing studies have shown that the components of nanotubes can be carbon, silicon dioxide, simple metals, and metal oxides. At present, the synthesis of nanotubes usually uses surfactants as templates, using chemical processes such as hydrolysis, crystallization, etching or extraction, through the interfacial interaction between templates and precursors and the self-assemb...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J32/00B01J31/06C07F17/02C07F7/18
Inventor 刘晓张胜波孙靖王华韩金玉
Owner TIANJIN UNIV
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