Tetrahydrofuran C-H multiphase oxidation method

A technology of tetrahydrofuran and potassium chloride, applied in the application field of organic matter conversion, can solve problems such as loss of activity, waste of catalyst, unstable catalyst, etc., and achieve the effects of mild reaction conditions and simple and easy preparation process.

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

AI Technical Summary

Problems solved by technology

However, most of them are based on homogeneous molecular catalysts. In this way, the catalysts are very unstable during the reaction, are easily oxidized and lose their activity, and are difficult to separate from the reaction system after the reaction, so that the c

Method used

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  • Tetrahydrofuran C-H multiphase oxidation method
  • Tetrahydrofuran C-H multiphase oxidation method
  • Tetrahydrofuran C-H multiphase oxidation method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] Step 1: Dissolve 0.875g KCl and 0.275g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO20-PO70-EO20 (P123) in 120mL of 1.8M hydrochloric acid solution, stir rapidly to make Form a uniform transparent solution, add 3.15mmol organosilane precursor 1,4-bis(triethoxysilyl)benzene and continue to stir vigorously, reduce the stirring speed and continue stirring, then add 0.35mmol bipyridine precursor 4,4'-[4 -(Trimethoxysilanyl)butyl]-2,2'-bipyridine was stirred at 30°C for 24h.

[0034] Step 2: Add the obtained white emulsion into a 100ml polytetrafluoroethylene liner and place it in a constant temperature drying oven at 70°C. After standing for 30 hours, filter it with a sand core funnel, and wash it with deionized water several times to ensure that the filtrate is No more air bubbles are produced. After the obtained product was dried and dehydrated at 20°C, it was extracted with ethanol and concentrated hydrochloric acid at 60°C (the extra...

Embodiment 2

[0038]Step 1: Dissolve 1.75g ​​KCl and 0.55g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO20-PO70-EO20 (P123) in 120mL 2M hydrochloric acid solution, stir rapidly to form Uniform and transparent solution, add 2.8mmol organosilane precursor 1,4-bis(triethoxysilyl)benzene and continue to stir vigorously, reduce the stirring speed and continue stirring, then add 0.7mmol bipyridine precursor 4,4'-[4 -(Trimethoxysilanyl)butyl]-2,2'-bipyridine was stirred at 35°C for 18h.

[0039] Step 2: Add the obtained white emulsion into a 100ml polytetrafluoroethylene liner and place it in a 90°C constant temperature drying oven. After standing for 25 hours, filter it with a sand core funnel, and wash it with deionized water several times to ensure that the filtrate No more air bubbles are produced. After the obtained product was dried and dehydrated at 50°C, it was extracted and refluxed at 70°C for 8 hours using ethanol and concentrated hydrochloric acid. ...

Embodiment 3

[0043] Step 1: Dissolve 3.5KCl and 1.1g triblock copolymer surfactant polyoxyethylene-polyoxypropylene-polyoxyethylene EO20-PO70-EO20 (P123) in 120mL of 2.2M hydrochloric acid solution, stir rapidly to make it Form a uniform transparent solution, add 2.45mmol organosilane precursor 1,4-bis(triethoxysilyl)benzene and continue to stir vigorously, reduce the stirring speed and continue stirring, then add 1.05mmol bipyridine precursor 4,4'-[ 4-(Trimethoxysilanyl)butyl]-2,2'-bipyridine was stirred at 40°C for 12h.

[0044] Step 2: Add the obtained white emulsion into a 100ml polytetrafluoroethylene liner, place it in a constant temperature drying oven at 110°C, let it stand for 20 hours, filter it with a sand core funnel, and wash it with deionized water several times to ensure that the filtrate does not contain Bubbles are generated again. After the obtained product was dried and dehydrated at 60° C., extraction and reflux were carried out at 80° C. for 6 h using ethanol and conc...

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Abstract

The invention relates to a tetrahydrofuran C-H multiphase oxidation method. 4,4'-[4-(trimethoxy silane) butyl]-2,2'-bipyridine is embedded into an organic silicon nanotube, and dichloro(pentamethylcyclopentadienyl) iridium dimer is coordinated into the nanotube to obtain an iridium-based bipyridine-organic silicon nanotube multiphase catalyst. The catalyst is mixed with tetrahydrofuran, and a reaction is performed at a normal temperature by taking sodium periodate as an oxidant and heavy water as a solvent. The catalyst has a clear porous structure, a large specific surface area and uniform active sites, and has a very good catalytic effect on tetrahydrofuran C-H oxidation, and because the catalyst has the characteristics of relatively high stability and easy recovery, the catalyst has a very good actual application prospect in industry.

Description

technical field [0001] The invention relates to a tetrahydrofuran C-H heterogeneous system oxidation technology, which belongs to the application in the transformation of organic matter. Background technique [0002] Tetrahydrofuran (THF), also known as 1,4-epoxybutylene, one oxygen pentacycline, etc., is a five-membered ring ether. Because its α-position hydrogen is more active, it is easily oxidized. The oxidation products of THF mainly include γ-butyrolactone, 2-hydroxytetrahydrofuran, 1,4-succinic acid, 4-hydroxybutyric acid, etc. Among them, γ-butyrolactone is the most widely used and is an important fine chemical and pharmaceutical intermediate. It is mainly used in the synthesis of pyrrolidone series products α-acetyl, γ-butyrolactone and the pharmaceutical intermediate cyclopropylamine. It is also used in agriculture. Chemistry, petrochemistry and other fields. At present, the annual consumption of γ‐butyrolactone in China is about 18,000 tons, of which the consum...

Claims

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Application Information

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IPC IPC(8): C07D307/20C07D307/33C07C51/31C07C55/10
CPCC07C51/31C07D307/20C07D307/33C07C55/10
Inventor 刘晓张胜波李梅王华韩金玉
Owner TIANJIN UNIV
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