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A kind of modified mesoporous silica adsorbent and its preparation method and application

A mesoporous silica and adsorbent technology, applied in chemical instruments and methods, silicon compounds, inorganic chemistry, etc., to achieve the effects of convenient operation, simple preparation process, and high grafting rate

Active Publication Date: 2019-01-18
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But so far, the reports on azamacrocyclic ligands mainly focus on the coordination model construction of transition metals and some heavy metals, while the coordination of noble metals, especially the selective separation of split palladium in high-level waste liquid, has not been reported yet.

Method used

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  • A kind of modified mesoporous silica adsorbent and its preparation method and application
  • A kind of modified mesoporous silica adsorbent and its preparation method and application
  • A kind of modified mesoporous silica adsorbent and its preparation method and application

Examples

Experimental program
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Effect test

Embodiment 1

[0029] Example 1: A preparation method of modified mesoporous silica adsorbent

[0030] Dissolve 3.5g of 1,4,7,10-tetraazacyclododecane (Cyclen), 4g of potassium iodide, and 10g of potassium carbonate in 150mL of anhydrous tetrahydrofuran. Porous silica (precursor chlorine-based functionalized mesoporous silica (SBA-15-Cl) preparation, refer to the relevant literature C.Yu, et al.Advanced Materials.14 (23) (2002) 1742), Reflux reaction under continuous stirring for 48 hours, after cooling to room temperature, the product was separated by suction filtration, washed alternately with ethanol and water several times, and vacuum-dried at 75°C for 12 hours to obtain a modified mesoporous silica adsorbent.

[0031] figure 1 (a) is the transmission electron microscope photo of mesoporous silica (SBA-15-Cl) functionalized with precursor chlorine groups, and the ordered pore structure can be clearly observed, and the pore diameter is about 10nm, which belongs to the mesoporous range; ...

Embodiment 2

[0033] Embodiment 2: the modified mesoporous silica adsorbent obtained in embodiment 1 is to the recovery of palladium in nitric acid medium

[0034]Pipette 20 mL of a 50 mg / L palladium solution with a nitric acid acidity of 0.1 mol / L in a conical flask, add 0.02 g of the modified mesoporous silica adsorbent obtained in Example 1, and after ultrasonication for 5 min, the Shake at 200r / min for 24h in a constant temperature air bath. After centrifuging the adsorbent, the remaining clear liquid was taken out, and the mass concentration of palladium was measured by atomic absorption spectroscopy, and the adsorption rate E=89.1% of palladium was calculated by the adsorbent according to the adsorption equilibrium formula.

Embodiment 3

[0035] Embodiment 3: the modified mesoporous silica adsorbent obtained in embodiment 1 is to the recovery of palladium in nitric acid medium

[0036] Pipette 20 mL of a 50 mg / L palladium solution with a nitric acid acidity of 0.5 mol / L in an Erlenmeyer flask, add 0.02 g of the modified mesoporous silica adsorbent obtained in Example 1, and after ultrasonication for 5 min, at 25 ± 0.2 ° C Shake at 200r / min for 24h in a constant temperature air bath. After centrifuging the adsorbent, the remaining clear liquid was taken out, and the mass concentration of palladium was measured by atomic absorption spectrometry, and the adsorption rate E=80.6% of the adsorbent to palladium was calculated according to the adsorption equilibrium formula.

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Abstract

The invention relates to a modified mesoporous silica adsorbent and a preparation method and application thereof. Under the catalysis of potassium carbonate and potassium iodide, aza-macrocyclic ligand is modified onto the surface of chlorine group functional mesoporous silica through nucleophilic substitution, and the adsorbent is prepared; palladium recycling and enrichment under different nitric acid concentrations are achieved through the adsorbent, and the selective recovery performance of palladium in highly-active effluent simulated feed liquid is evaluated. According to the modified mesoporous silica adsorbent, mesoporous nanomaterials are combined with the supermolecule recognition performance of the aza-macrocyclic ligand, the problems that selectivity is poor, operation is complex, the raw material cost is high and the stability is poor in the traditional treatment technology for palladium in highly-active effluent are solved, and the adsorbent has the advantages of being good in selectivity, large in adsorption capacity, high in adsorption speed and easy to recycle for palladium within the wide nitric acid concentration range, and has the great practical significance in the aspects of nuclear fuel reprocessing and hydrometallurgy.

Description

technical field [0001] The invention belongs to the technical field of resource utilization and environmental protection, and in particular relates to a modified mesoporous silica adsorbent and its preparation method and application. Background technique [0002] As a rare precious metal, palladium is widely used in the fields of catalysis, medicine and electrical component manufacturing due to its unique physical and chemical properties. However, the content of palladium in nature is extremely low (≈10 -6 ), and the distribution is uneven, the extraction is difficult, and it is difficult to meet the growing needs of people. In addition, the chemical and biological toxicity of palladium also constitutes a potential hazard to human activities and the biological environment. Therefore, finding new palladium resources and establishing economical, green, and environmentally friendly separation methods to achieve sustainable utilization of palladium have always been the focus o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J20/10B01J20/30C22B11/00C22B7/00
CPCB01J20/103C22B7/006C22B11/046Y02P10/20
Inventor 陈靖吴奉承叶钢
Owner TSINGHUA UNIV
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