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Magnetic solid-phase separating agent and method for preparing same

A phase separation agent, magneto-solid technology, applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve product polymerization inhibitor residues, unfavorable large-scale production, complex preparation methods, etc. problem, to achieve the effect of stable reaction system, easy automation and good repeatability

Active Publication Date: 2012-08-15
SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to overcome the disadvantages of the existing preparation method of magnetic solid phase separation agent, such as complex preparation method due to the inclusion of polymerization steps, residual polymerization inhibitor in the product, difficult control of the product, and unfavorable for large-scale production. A new magnetic solid-phase separation agent and its preparation method are provided. The preparation method is suitable for large-scale production. The magnetic solid-phase separation agent has the characteristics of high efficiency, high selectivity and strong magnetic response, and can greatly shorten the separation time

Method used

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  • Magnetic solid-phase separating agent and method for preparing same
  • Magnetic solid-phase separating agent and method for preparing same
  • Magnetic solid-phase separating agent and method for preparing same

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0038] Example 1 Fe 3 o 4 Preparation method of magnetic nanoparticles:

[0039] Prepare 1250ml 0.5M NaOH and 125ml 1M FeCl respectively 3 , 125ml 0.5M FeCl 2 and 125ml 0.4M HCl solution, NaOH solution in N 2 Heating to 60°C under protective conditions, the prepared FeCl 3 , FeCl 2 After mixing with HCl solution, mix with NaOH, stir vigorously at 100 rpm for 15 min and cool to room temperature. Washed 5 times with deionized water and methanol successively, the resulting product Fe 3 o 4 Magnetic nanoparticles are dispersed in methanol; the magnetic properties of the product are detected, and the obtained hysteresis curve is as follows figure 2 shown.

Embodiment 2

[0040] Embodiment 2 Preparation method of silanized magnetic particles:

[0041] The gamma-Fe that is dispersed in the methanol that makes in embodiment 1 3 o 4 After removing methanol from the magnetic nanoparticles, weigh 20g and add it to a mixed solvent of 1000ml toluene and methanol (the volume ratio of toluene to methanol is 1:1), add 100ml tetraethyl orthosilicate (TEOS), heat up to 80°C, and pass through N 2 , stirred vigorously at a speed of 300rpm, and after refluxing for 24h, washed 6 times with toluene to obtain silanized magnetic nanoparticles, and dispersed in toluene; the TEM of the obtained silanized magnetic nanoparticles was as follows: figure 1 Shown, XRD as image 3 shown.

Embodiment 3

[0042] The preparation method of the magnetic nanoparticles modified by the amino group of embodiment 3:

[0043] Add 20 g of the alkylated magnetic nanoparticles prepared in Example 2 into 600 ml of a mixed solvent of toluene and methanol (the volume ratio of toluene and methanol is 1:1), and add 20 ml of silane coupling agent (AEAPS). Heating to 50°C, passing through N 2 , stirred at a speed of 300 rpm, and refluxed for 24 hours, washed with toluene, methanol, and aqueous solution several times in sequence to obtain amino-modified magnetic nanoparticles, and dried.

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Abstract

The invention provides a method for preparing a magnetic solid-phase separating agent. The method comprises the following steps of: in solution of non-protonic non-polar solvent and under an action of a dehydrating agent of dicyclohexylcarbodiimide, subjecting amino group-modified magnetic nano particles and carboxyl group-containing crown ether to a dehydration reaction of amino groups and carboxyl groups. The invention also provides a magnetic solid-phase separating agent prepared by the method. Aiming at overcoming the defect that because a polymerization step is included, the preparation method is complicated, a polymerization inhibitor is remained in products, the products are difficult to control, mass production cannot be conveniently realized and other defects existing in the conventional method for preparing the magnetic solid-phase separating agent, the invention provides the magnetic solid-phase separating agent and the preparation method thereof, wherein the preparation method is suitable for mass production; and the magnetic solid-phase separating agent has the characteristics of high effectiveness, high selectivity, strong magnetic response, short separation time andthe like.

Description

technical field [0001] The invention relates to a magnetic solid phase separation agent and a preparation method thereof. Background technique [0002] Magnetically assisted chemical separation [magnetically assisted chemical separation (MACS)] method is a practical method that combines chemical adsorbents with high selectivity for the target with magnetic particles that can be collected by a magnetic field, thereby separating the target by a magnetic field , the method was early developed in Argonne National Laboratory (ANL, USA). At present, the selected chemical adsorbents are mostly extractants and ion exchangers, that is, MACS combined with extractants / ion exchangers, and then magnetic separation can obtain good chemical separation effects. MACS has three advantages: ①Compared with solvent extraction and ion exchange, it rarely uses complex equipment; ②It can easily increase the amount of separating agent, thereby improving the separation efficiency; ③It can be used in...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30
Inventor 张国欣王妮张岚刘静培李潇沈华
Owner SHANGHAI INST OF APPLIED PHYSICS - CHINESE ACAD OF SCI