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Method for extracting and separating palladium ions through pillar arene ramification

A technology of derivatives and pillar aromatics, which is applied in the field of extracting and separating palladium ions by using pillar aromatic derivatives, can solve the problems of not finding a high-efficiency recovery path, long radioactive cycle, high radioactivity, etc., and achieves easy operation, strong selectivity, The effect of efficient separation

Inactive Publication Date: 2016-06-15
ZHEJIANG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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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 for extracting and separating palladium ions through pillar arene ramification
  • Method for extracting and separating palladium ions through pillar arene ramification
  • Method for extracting and separating palladium ions through pillar arene ramification

Examples

Experimental program
Comparison scheme
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 solv...

Embodiment 2

[0043] A preparation method of pillar arene derivatives, comprising:

[0044] (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.

[0045] Wherein, the molar ratio of 1,4-p-methoxybenzene and paraformaldehyde is 1:2, the molar ratio of 1,4-p-methoxybenzene and catalyst boron trifluoride ether is 1:1.1, and the reaction temperature is 29° C., the reaction time is 3 minutes, and the amount of solvent used is 8 ml per mmol of 1,4-p-methoxybenzene.

[0046] (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.

[0047] Wherein, the molar ratio of permethoxycolum[5]arene to boron tribromide is 1:22, the reaction temperature is 30°C, the reaction time is 3 days, and the amount of sol...

Embodiment 3

[0051] A preparation method of pillar arene derivatives, comprising:

[0052] (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.

[0053] Wherein, the molar ratio of 1,4-p-methoxybenzene and paraformaldehyde is 1:4, the molar ratio of 1,4-p-methoxybenzene and catalyst boron trifluoride ether is 1:1.2, and the reaction temperature is 30° C., the reaction time is 3 minutes, and the amount of solvent used is 10 ml per mmol of 1,4-p-methoxybenzene.

[0054] (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.

[0055] Wherein, the molar ratio of permethoxypyrro[5]arene to boron tribromide is 1:25, the reaction temperature is 35°C, the reaction time is 4 days, and the amount of so...

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Abstract

The invention discloses a method for extracting and separating palladium ions through a pillar arene ramification. A dichloromethane solution or a chloroform solution containing an extraction agent serves as an organic phase, the concentration of the extraction agent in the organic phase ranges from 0.01 M to 0.02 M, and after the organic phase and a nitric acid aqueous solution containing various metal ions are mixed, the mixture is vibrated, wherein the vibration temperature is 25+ / -1 DEG C, and the vibration time ranges from 85 h to 100 h. The concentration of the various metal ions in the nitric acid aqueous solution ranges from 5*10-4 M to 1*10-2 M. The concentration of HNO3 in the nitric acid aqueous solution ranges from 0.4 M to 9 M. According to the method for extracting and separating palladium ions through the pillar arene ramification, the efficient separation of the palladium element can be conducted, the process is simple, and operation is easy.

Description

technical field [0001] The invention relates to the technical field of separation of palladium, in particular to a method for extracting and separating palladium ions by using pillar aromatic hydrocarbon derivatives. 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 expensi...

Claims

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Application Information

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IPC IPC(8): C22B11/00C22B3/36
CPCC22B11/04C22B3/362Y02P10/20
Inventor 张安运何敏清
Owner ZHEJIANG UNIV
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