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Iridium based dipyridine-organic silicon nanotube heterogeneous catalyst and preparation method thereof

A technology based on bipyridine and organosilicon, which is applied in the field of iridium-based bipyridine-organosilicon nanotube heterogeneous molecular catalyst and preparation, can solve the problems of difficulty in recycling, industrial application limitation, poor stability of homogeneous molecular catalyst, etc. Stability, lower requirements for equipment, easy recovery and recyclable effects

Inactive Publication Date: 2017-04-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Benefits of technology

This patented technology allows for creation of an improved type of material called silica based on iridum (Ir) atoms that could hold many types of chemical reactions like hydrogenation or oxo reduction. These materials had wide applications ranging from electronics to biology. They found their unique properties when used alone without other substances such as water vapor or oxygen during use. By adding certain elements into these structures, they made them stronger than usual metals while still being easier to manufacture at lower costs compared to existing methods.

Problems solved by technology

Technological Problem: Current methods for creating stable and recoverable solid state mesoporial structures (SSM) involve expensive procedures like template preparations or solvent evaporation techniques.

Method used

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  • Iridium based dipyridine-organic silicon nanotube heterogeneous catalyst and preparation method thereof
  • Iridium based dipyridine-organic silicon nanotube heterogeneous catalyst and preparation method thereof
  • Iridium based dipyridine-organic silicon nanotube heterogeneous catalyst and preparation method thereof

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Experimental program
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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. Then 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 homogeneous transparent solution, added 3.15mmol organosilane precursor 1,4‐bis(triethoxysilyl)benzene and continued to stir vigorously, reducing the stirring rate Continue to stir...

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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PUM

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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

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Claims

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Application Information

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Owner TIANJIN UNIV
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