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A kind of magnetic adsorbent and preparation method thereof and recovery of palladium in nitric acid medium

A magnetic adsorbent, nitric acid technology, applied in the direction of selective adsorption, chemical instruments and methods, radioactive purification, etc., to achieve the effect of fast adsorption rate, good superparamagnetic performance, and high separation efficiency

Active Publication Date: 2019-02-22
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, the coordination of azamacrocyclic carboxylic acid derivatives to noble metals, especially the rapid separation of split palladium in high-level waste, has not been reported.

Method used

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  • A kind of magnetic adsorbent and preparation method thereof and recovery of palladium in nitric acid medium
  • A kind of magnetic adsorbent and preparation method thereof and recovery of palladium in nitric acid medium
  • A kind of magnetic adsorbent and preparation method thereof and recovery of palladium in nitric acid medium

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1: a kind of preparation method of magnetic adsorbent, comprises the following steps:

[0033](1) Dissolve 1.0 mmol of azamacrocyclic carboxylic acid derivative 1,4,7,10-tetraazacyclododecane-1,4,7,10-tetraacetic acid (DOTA) in 50 mL of morpholinoethanesulfonate In the acid biological buffer solution, adjust the pH buffer between 5.4 to 5.5, under the protection of nitrogen, add the catalyst 25.0mmol EDC·HCl and 10mmol NHS, stir and react at room temperature for 1h, and prepare the activated intermediate of the azamacrocyclic carboxylic acid derivative DOTA .

[0034] (2) Add 0.5 g of amino-functionalized magnetic microspheres to the above reaction solution (for the preparation of amino-functionalized magnetic microspheres, refer to relevant literature Wang Xiangke, et al. Chemical Engineering Journal. 2014, 235, 275-283), and ultrasonically disperse Finally, first react at 25±0.2°C for 8 hours under the action of mechanical stirring, then cool to 4±0.2°C an...

Embodiment 2

[0037] Embodiment 2: the magnetic adsorbent of embodiment 1 gained is to the recovery of palladium in the nitric acid medium

[0038] Pipette 10 mL of a 50 mg / L palladium solution with a nitric acid acidity of 0.01 mol / L in a conical flask, add 0.1 g of the magnetic adsorbent obtained in Example 1, and after ultrasonication for 5 min, in a constant-temperature air bath at 25 ± 0.2 ° C at 200 r / min oscillation for 24h. After the magnet separates the adsorbent, take out the supernatant, measure the mass concentration of palladium in it with atomic absorption spectrometry, and calculate the adsorption rate E=99.8% of the adsorbent to palladium at this moment according to the adsorption equilibrium formula.

Embodiment 3

[0039] Embodiment 3: the magnetic adsorbent of embodiment 1 gained is to the recovery of palladium in the nitric acid medium

[0040] Pipette 10 mL of a 50 mg / L palladium solution with an acidity of nitric acid of 0.1 mol / L in a conical flask, add 0.1 g of the magnetic adsorbent obtained in Example 1, and after ultrasonication for 5 min, in a constant-temperature air bath at 25 ± 0.2 ° C at 200 r / min oscillation for 24h. After the magnetic separation adsorbent, take out the supernatant, measure the mass concentration of palladium wherein with atomic absorption spectrometry, calculate this adsorbent to the adsorption rate E=98.2% of palladium now according to the adsorption equilibrium formula.

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Abstract

The invention relates to a magnetic adsorbent as well as a preparation method thereof, and recycling of palladium in a nitric acid medium. Through amidation catalyzed by EDC.HCL and NHS, a polyaza polycarboxylic acid derivative is modified on the outer surface of an amino-functionalized magnetic microsphere, and a core-shell structure adsorbent, provided with a Fe3O4 magnetic nanoparticle as a core, SiO2 as a protective shell, and the polyaza polycarboxylic acid derivative modified on the outer edge of the shell, is prepared. The preparation technology has the advantages of low energy consumption, low cost and simple operation. The magnetic adsorbent has large palladium adsorption capacity and high adsorption rate in a relatively wide nitric acid concentration range; even under interference from various high-level liquid waste fission product nuclides, the magnetic adsorbent exerts excellent selective separation ability; however, palladium absorbed on the surface of the adsorbent can be eluted by a nitric acid solution containing 5% thiourea, thereby facilitating recycling.

Description

technical field [0001] The invention belongs to the technical field of resource utilization and environmental protection, and in particular relates to a magnetic adsorbent, a preparation method thereof and recovery of palladium in nitric acid medium. Background technique [0002] In the contemporary era of energy and the environment, with the increasingly serious problems of the greenhouse effect and smog pollution, actively developing nuclear energy with high energy density, clean and low carbon can not only effectively improve the energy structure, relieve environmental pressure, but also help safeguard National energy and economic security. According to my country's medium and long-term nuclear power development plan (National Development and Reform Commission. Nuclear Power Medium and Long-term Development Plan 2005-2020, 2007.), by 2020, China's installed nuclear power capacity will reach 58 million kilowatts, and 30 million kilowatts are under construction. However, a...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/22B01J20/28B01J20/30B01D15/08G21F9/12C22B7/00C22B11/00
CPCB01D15/08B01J20/06B01J20/103B01J20/22B01J20/28009B01J2220/46B01J2220/4806B01J2220/4812C22B11/042G21F9/12Y02P10/20
Inventor 陈靖吴奉承叶钢
Owner TSINGHUA UNIV