Chiral magnetic nano-particles and preparation and application thereof

A magnetic nanoparticle and nanoparticle technology, applied in chemical instruments and methods, organic racemization, organic chemistry, etc., to achieve the effects of good separation effect, simple and convenient operation, and short separation time

Inactive Publication Date: 2011-01-12
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The study of derivatizing cellulose and binding it to the surface of magnetic particles to exert its chiral separation performance has not been reported

Method used

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  • Chiral magnetic nano-particles and preparation and application thereof
  • Chiral magnetic nano-particles and preparation and application thereof
  • Chiral magnetic nano-particles and preparation and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Fe 3 o 4 Preparation of Magnetic Nanoparticles: FeCl 3 .6H 2 O (2.0g) and FeCl 2 .4H 2 O (1.0g) is dissolved in water according to the amount of substance 1.5:1, pass through N 2 After 20 minutes, the temperature was raised to 60°C, and NH was added dropwise to the solution 3 .H 2 O to adjust pH=9, stop the reaction after 0.5h of heat preservation reaction, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water until pH=7, vacuum dry at 60°C and grind to obtain the product Fe 3 o 4 stand-by;

[0024] (2) Fe 3 o 4 / SiO 2 Preparation of composite magnetic nanoparticles: weighing the first step product Fe 3 o 4 1g, add H 2 O and EtOH (1:1, v / v) 60ml ultrasonic dispersion 10min, pass N 2 , add NH under stirring 3 .H 2 O to adjust the pH to 9, add 1ml TEOS to the solution after heating up, keep it warm for 8 hours, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water an...

Embodiment 2

[0030] (1) Fe 3 o 4 Preparation of Magnetic Nanoparticles: FeCl 3 .6H 2 O (2.1g) and FeCl 2 .4H 2 O (1.0g) is dissolved in water according to the amount of substance 1.6:1, pass through N 2 After 30 minutes, the temperature was raised to 70°C, and NH was added dropwise to the solution 3 .H 2 O to adjust pH=9, stop the reaction after 0.5h of heat preservation reaction, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water until pH=7, vacuum dry at 70°C and grind to obtain the product Fe 3 o 4 stand-by;

[0031] (2) Fe 3 o 4 / SiO 2 Preparation of composite magnetic nanoparticles: weighing the first step product Fe 3 o 4 1g, add H 2 O and EtOH (1:1, v / v) 80ml ultrasonic dispersion 20min, pass N 2 , add NH under stirring 3 .H 2 O to adjust the pH to 9, add 1ml TEOS to the solution after heating up, keep it warm for 9 hours, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water an...

Embodiment 3

[0037] (1) Fe 3 o 4 Preparation of Magnetic Nanoparticles: FeCl 3 .6H 2 O (2.4g) and FeCl 2 .4H 2 O (1.0g) is dissolved in water according to the amount of substance 1.75:1, pass through N 2 After 30 minutes, the temperature was raised to 70°C, and NH was added dropwise to the solution 3 .H 2 O to adjust pH=9, stop the reaction after 0.5h of heat preservation reaction, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water until pH=7, vacuum dry at 60°C and grind to obtain the product Fe 3 o 4 stand-by;

[0038] (2) Fe 3 o 4 / SiO 2 Preparation of composite magnetic nanoparticles: weighing the first step product Fe 3 o 4 1g, add H 2 O and EtOH (1:2, v / v) 60ml ultrasonic dispersion 30min, pass N 2 , add NH under stirring 3 .H 2 Adjust O to pH=9, add 1.5ml TEOS to the solution after heating up, keep warm for 8 hours, transfer the reaction mixture to a centrifuge tube for centrifugation, wash with deionized water and EtOH,...

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Abstract

The invention relates to chiral magnetic nano-particles and preparation and application thereof. The preparation comprises the following steps of: (1) preparing Fe3O4 magnetic nano-particles; (2) preparing Fe3O4/SiO2 composite magnetic nano-particles; (3) preparing cellulose-2,3-di(3,5-dimethyl phenyl carbamate); and (4) performing surface chiral modification on the Fe3O4/SiO2 composite magnetic nano-particles by using the cellulose-2,3-di(3,5-dimethyl phenyl carbamate). The chiral magnetic nano-particles are used for separating a racemic compound DL-1-phenethyl alcohol, and an optical rotation value test for obtaining components through singly spinning a guide sample and separation proves that laevo-rotation and dextro-rotation are separated very well. The chiral magnetic nano-particles have the advantages of short separation time, simple and convenient operation, and good separation effect of chiral compounds; besides, the chiral magnetic nano-particles can be thoroughly separated from base solution under an external magnetic field, and not only cannot cause pollution to a target separation object but also can be completely recycled, thereby fulfilling two aims of ecumenical efficiency and environmental protection.

Description

technical field [0001] The invention relates to a magnetic nano particle and its preparation and application. Background technique [0002] Chiral issues are closely related to our daily life, and the separation of chiral compounds, especially chiral drugs, has received more and more attention. At present, the separation methods of chiral compounds mainly focus on the development of chromatographic chiral stationary phases and chiral additives. Many chiral compounds for liquid chromatography have been developed, mainly polysaccharide derivatives, cyclodextrins and proteins, etc., but these separations have extremely high requirements on instrument performance and material purity, are expensive, time-consuming, and difficult Recycling is prone to problems such as waste and pollution, so the development of more efficient chiral separation materials is crucial. Nano-magnetic materials refer to quasi-zero-dimensional ultrafine powders, one-dimensional ultra-thin films or two-d...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08B15/06C07B57/00C07C33/22C07C29/76
Inventor 魏芸田爱林
Owner BEIJING UNIV OF CHEM TECH
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