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Preparation method of nitroxide radical spinning probe with surface activity

A nitroxide radical and surface active technology, applied in the direction of organic chemistry, can solve the problems of inconvenience, the lack of surface activity of nitroxide radical spin probe, increase the cost of use, etc., and achieve the effect of convenient separation and purification

Active Publication Date: 2018-05-29
XI'AN PETROLEUM UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] Most of the above two nitrogen-oxygen radical spin probes have no surface activity, and they need to be used in conjunction with surfactants during use, which increases the cost of use and brings some inconvenience to the actual use process

Method used

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  • Preparation method of nitroxide radical spinning probe with surface activity
  • Preparation method of nitroxide radical spinning probe with surface activity
  • Preparation method of nitroxide radical spinning probe with surface activity

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] This embodiment is realized through the following steps:

[0028] (1), preparation of intermediate-dodecyl alcohol polyoxyethylene ether (m=9) chloride

[0029] Add 0.0205mol dodecyl alcohol polyoxyethylene ether (m=9) and 0.0369mol pyridine into a 100mL three-necked flask equipped with a stirrer, reflux condenser, and thermometer, stir evenly and slowly add 0.0369mol thionyl chloride dropwise, Stir the reaction at 60-70°C for 10 hours, stop the reaction, cool, and let it stand, the organic matter in the upper layer is neutralized with 15% sodium hydroxide solution to pH ≥ 7, and then transferred to a separatory funnel to separate the water layer, and the organic layer is washed with water for 5 -6 times, until there is no irritating smell; then pour it into a single-necked round bottom flask, add 50ml of petroleum ether (60-90°C), reflux with a water separator to remove water, and then distill the petroleum ether to obtain a brown transparent liquid .

[0030] Depend...

Embodiment 2

[0036] This embodiment is realized through the following steps:

[0037] (1), preparation of intermediate-octylphenol polyoxyethylene ether (m=10) chloride

[0038] Add 0.0205mol octylphenol polyoxyethylene ether (m=10) and 0.0369mol pyridine into a 100mL three-necked flask equipped with a stirrer, reflux condenser, and thermometer, stir evenly, and slowly add 0.0369mol thionyl chloride dropwise, Stir the reaction at 60-70°C for 10 hours, stop the reaction, cool, and let it stand, the organic matter in the upper layer is neutralized with 15% sodium hydroxide solution to pH ≥ 7, and then transferred to a separatory funnel to separate the water layer, and the organic layer is washed with water for 5 -6 times, until there is no irritating smell; then pour it into a single-necked round bottom flask, add 50ml of petroleum ether (60-90°C), reflux with a water separator to remove water, and then distill the petroleum ether to obtain a brown transparent liquid .

[0039] (2), prepar...

Embodiment 3

[0043] This embodiment is realized through the following steps:

[0044] (1), preparation of intermediate-fatty alcohol polyoxypropylene ether (n=15) chloride

[0045] Add 0.0205mol fatty alcohol polyoxypropylene ether (n=15), 0.0369mol pyridine in a 100mL three-necked flask equipped with a stirrer, reflux condenser, and thermometer, and slowly add 0.0369mol thionyl chloride dropwise after stirring evenly. Stir and react at 60-70°C for 3.5 hours, stop the reaction, cool, and let stand, and neutralize the organic matter in the upper layer with 15% sodium hydroxide solution to pH ≥ 7, transfer it into a separatory funnel to separate the water layer, and wash the organic layer with water for 5- 6 times until there is no irritating smell; then pour it into a single-necked round bottom flask, add 50ml of petroleum ether (60-90°C), reflux with a water separator to remove water, and then distill the petroleum ether to obtain a brown transparent liquid.

[0046](2), preparation of su...

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Abstract

The invention relates to a preparation method of a nitroxide radical spinning probe with surface activity. The preparation method comprises the steps of allowing a non-ionic surfactant to react with thionyl chloride in a pyridine solvent to synthesize non-ionic surface active chloride as an intermediate, performing purification and refining, allowing the chloride to react with 4-hydroxyl-2,2,6,6-tetramethyl piperidine nitroxide radical and an active alkali metal or a hydride of the active alkali metal in a tetrahydrofuran solvent to form sodium alkoxide salt for reaction, and synthesizing thenitroxide radical spinning probe with the surface activity. The nitroxide radical spinning probe integrates a spinning characteristic and surface activity. The piperidine nitroxide radical is bonded with a terminal hydroxyl group of the non-ionic surfactant by a molecular design. Therefore, the probe has the spinning characteristic in addition to the intrinsic surface activity.

Description

technical field [0001] The invention relates to the field of spin probes in chemistry, in particular to a method for preparing a surface-active nitroxide free radical spin probe. Background technique [0002] In order to study the catalytic effect of chemical reactions in colloidal systems, the microstructure of emulsions, and the microstructure of biofilms in biochemistry, people usually use the method of introducing spin probes, using electron spin resonance spectroscopy for detection, and ESR The changes and parameters of the spectral characteristic spectrum, so as to indirectly understand the microscopic information in this regard. [0003] The nitroxide radical probe is one of the commonly used spin probes. Nitroxide radical probes are generally divided into two types: water-soluble spin probes and partially water-soluble spin probes. Water-soluble nitroxide free radical probes include: 2,2,6,6-tetramethyl-4-hydroxypiperidine-1-oxyl radical, 2,2,6,6-tetramethyl-4-amin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G65/333C08G65/334C07D211/94
CPCC07D211/94C08G65/33396C08G65/3344
Inventor 张科良
Owner XI'AN PETROLEUM UNIVERSITY
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