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Magnetic solid-phase separating agent and method for preparing same

A phase separation agent and magnetic solidification technology, applied in chemical instruments and methods, other chemical processes, alkali metal oxides/hydroxides, etc., can solve the problem of product inhibitor residue, unfavorable large-scale production, difficult product control, etc. problem, to achieve the effect of stable reaction system, easy automation and good repeatability

Active Publication Date: 2010-08-11
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

Examples

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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, the NaOH solution in N 2 Heat to 60℃ under protective conditions, and remove the prepared FeCl 3 , FeCl 2 After mixing with HCl solution, mixing with NaOH, stirring vigorously at 100 rpm for 15 minutes, and cooling to room temperature. Wash with deionized water and methanol for 5 times in turn, the resulting product Fe 3 O 4 Magnetic nanoparticles are dispersed in methanol; the magnetic properties of the product are tested, and the hysteresis curve obtained is as follows figure 2 Shown.

Embodiment 2

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

[0041] Γ-Fe dispersed in methanol prepared in Example 1 3 O 4 After removing methanol from the magnetic nanoparticles, weigh 20g and add it to 1000ml of mixed solvent of toluene and methanol (volume ratio of toluene to methanol 1:1), add 100ml of tetraethylorthosilicate (TEOS), heat up to 80℃, and pass in N 2 , Stir vigorously at 300 rpm, reflux for 24 hours, wash 6 times with toluene to obtain silanized magnetic nanoparticles, and disperse them in toluene; the TEM of the obtained silanized magnetic nanoparticles is as figure 1 As shown, XRD is as image 3 Shown.

Embodiment 3

[0042] Example 3 Preparation method of amino-modified magnetic nanoparticles:

[0043] 20 g of the alkylated magnetic nanoparticles prepared in Example 2 was added to 600 ml of a mixed solvent of toluene and methanol (toluene to methanol volume ratio 1:1), and 20 ml of silane coupling agent (AEAPS) was added. Heat to 50℃, pass in N 2 , Stirring at 300 rpm, refluxing for 24 hours, washing with toluene, methanol, and aqueous solution several times to obtain amino-modified magnetic nanoparticles, and drying.

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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 and the 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 (MACS) method is a practical method of combining a chemical adsorbent with high efficiency and selectivity for the target and magnetic particles that can be collected by a magnetic field, thereby separating the target by a magnetic field This method was developed in Argonne National Laboratory (ANL, USA) in the early stage. At present, most of the selected chemical adsorbents are extractants and ion exchangers, that is, MACS combined with extractant / ion exchanger, and then magnetic separation can obtain good chemical separation effect. MACS has three advantages: ①Compared with solvent extraction and ion exchange, it rarely uses complicated equipment; ②It can increase the amount of separating agent simply and conveniently, thereby improving the separation efficiency; ③It can be used in a w...

Claims

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Application Information

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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