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Method of adsorbing and separating palladium with high-molecular-based pillararene

An adsorption separation, polymer-based technology, applied in chemical instruments and methods, improvement of process efficiency, and other chemical processes, can solve the problems of long radioactive cycle, high content, and great harm, and achieve fast separation speed and selectivity Good, simple operation effect

Inactive Publication Date: 2016-08-10
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The high-level liquid waste (HLLW) produced by the reprocessing of spent fuel is a mixed solution of high acidity, high radioactivity and high toxicity, which contains a certain amount of Pd 107 , the half-life of palladium is 6.5×10 6 Years, the radioactive period is long, the hazard is great, and the content is high. It is of great significance if it can be recycled. However, at this stage, the separation of palladium in high-level radioactive waste liquid is still in the research stage, and no efficient recycling method has been found.

Method used

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  • Method of adsorbing and separating palladium with high-molecular-based pillararene
  • Method of adsorbing and separating palladium with high-molecular-based pillararene

Examples

Experimental program
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Effect test

Embodiment 1

[0034] A preparation method of pillar arene derivatives, comprising:

[0035] (1) 1,4-p-methoxybenzene and paraformaldehyde are reacted under the conditions of boron trifluoride ether as a catalyst and dry dichloromethane or 1,2-dichloroethane as a solvent to obtain permethoxy Pillar[5]arenes.

[0036] Wherein, the molar ratio of 1,4-p-methoxybenzene and paraformaldehyde is 1:1, the molar ratio of 1,4-p-methoxybenzene and catalyst boron trifluoride ether is 1:1, and the reaction temperature is 28°C, the reaction time is 3 minutes, and the amount of solvent used is 5 mL per mmoL of 1,4-p-methoxybenzene.

[0037] (2) Using the permethoxypyrro[5]arene obtained in step (1) as a raw material, react with boron tribromide under the condition of dry chloroform as a solvent to obtain perhydroxypyrro[5]arene.

[0038] Wherein, the molar ratio of permethoxycolumn[5]arene to boron tribromide is 1:20, the reaction temperature is 25°C, the reaction time is 2 days, and the amount of solven...

Embodiment 2

[0043] The commercially available ion exchange resin XAD-7 is activated as follows:

[0044] Weigh a certain amount of commercially available product XAD-7 into a 250mL round-bottomed flask, add an appropriate amount of methanol, stir at room temperature for 24 hours and then filter with suction. Store in a dry box.

Embodiment 3

[0046] Weigh 2.5g of the compound prepared in Example 1 in a 250mL round-bottomed flask, add 150mL of dichloromethane, add 10g of XAD-7 activated in Example 2 under stirring, move the system into a water bath, and place in a rotary evaporator After rotating and stirring at 45 °C for 120 min, the temperature was raised to 65 °C, and rotating and stirring for 180 min until the mixture was a loose powder. During this process, the perbutyrate-substituted pillar[5]arene derivatives entered the pores of the XAD-7 support by capillary action, and were finally vacuum-dried at 45 °C overnight to obtain a pink, loose adsorbent.

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PUM

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Abstract

The invention discloses a method of adsorbing and separating palladium with high-molecular-based pillararene. The method includes a step of mixing an adsorbent with a nitrate solution containing various metal ions, wherein the palladium ion is adsorbed and separated by the adsorbent. The adsorbent is prepared by supporting the compound represented as the structure formula (I) on a carrier, wherein 1 g of the adsorbent is mixed with 20-30 ml of the nitrate solution. The carrier is medium-polarity macroporous resin. Concentration of nitric acid in the nitrate solution is 0.4-8 M. The method of adsorbing and separating palladium with the high-molecular-based pillararene is free of addition of other organic compounds, has good selectivity, is high in separation speed, is easy to operate and is easy to promote.

Description

technical field [0001] The invention relates to the technical field of palladium element separation, in particular to a method for adsorbing and separating palladium by using polymer-based pillar aromatic hydrocarbons. Background technique [0002] The precious metal palladium has a special structure and has a special adsorption capacity for hydrogen and oxygen, so it occupies an irreplaceable position in the field of industrial catalysis. [0003] In addition to its excellent catalytic activity, palladium can maintain chemical inertness in a wide temperature range and has the characteristics of high melting point, friction resistance, corrosion resistance, strong ductility, and strong thermoelectric stability. It is widely used in national industries. each field. [0004] At present, my country's palladium resource reserves are limited and the output is very low, which is far from meeting the needs of the modern chemical industry. Most of them rely on imports and are expen...

Claims

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Application Information

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IPC IPC(8): C22B3/24C22B11/00B01J20/22B01J20/26
CPCB01J20/22B01J20/265C22B3/24C22B11/04Y02P10/20
Inventor 张安运王一宁
Owner ZHEJIANG UNIV
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