Extracting agent for nuclear waste liquid and preparation method for extracting agent

A technology of extractant and nuclear waste liquid, which is applied in the field of nuclear waste liquid extractant and its preparation, can solve the problems of low yield, difficulty in separation and purification, and limitation of large-scale application, and achieve the goal of increasing conversion rate and simplifying the separation process Effect

Inactive Publication Date: 2012-04-25
XI AN JIAOTONG UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

And because the tert-butyl group on 4', 4"(5")-di-tert-butyldibenzo-18-crown-6 benzene ring has extremely high lipophilicity, 4', 4"(5")-di The separation and purification of tert-butyldi...

Method used

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  • Extracting agent for nuclear waste liquid and preparation method for extracting agent
  • Extracting agent for nuclear waste liquid and preparation method for extracting agent
  • Extracting agent for nuclear waste liquid and preparation method for extracting agent

Examples

Experimental program
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Effect test

Embodiment 1

[0022] a. Weigh 6.2 g (0.05 mol) of p-methylcatechol and 32.5 g (0.1 mol) of cesium carbonate and dissolve them in 200 ml of tetrahydrofuran, wherein the cesium carbonate is added in two equal amounts. Weigh 0.05 mol of diethylene glycol xylene sulfonate, dissolve in 100 ml of tetrahydrofuran twice, and add dropwise in a constant pressure dropping funnel. The reaction was carried out at 40°C for 24 hours, and the reaction conversion rate was 26.3%.

[0023] b. Filtrate the mixture obtained by reacting according to the above step a, and distill under reduced pressure. Take 5g of the mixture, add 500g of γ-alumina and 500ml of n-heptane, reflux and co-heat the reaction at 60°C for 6h, filter the filtrate, and vacuum distill the filtrate. Recrystallization gave 4', 4"-dimethyldibenzo-18-crown-6( image 3 ), yield 50.5%, purity 73.6%.

Embodiment 2

[0025] a. Weigh 6.2 g (0.05 mol) of p-methylcatechol and 65 g (0.2 mol) of cesium carbonate and dissolve them in 300 ml of tetrahydrofuran, wherein the cesium carbonate is added in two equal amounts. Weigh 0.075 mol of diethylene glycol xylene sulfonate and dissolve it in 200 ml of tetrahydrofuran in two equal amounts, and add dropwise in a constant pressure dropping funnel. The reaction was carried out at 60°C for 60 hours, and the reaction conversion rate was 57.6%.

[0026] b. Filter the mixture obtained according to the above step a, weigh 5g of the mixture after vacuum distillation, add 300g of gamma alumina and 300ml of n-heptane, reflux at 70°C for 4h, filter and take the filtrate, and vacuum distill the filtrate. Recrystallization gave 4', 4"-dimethyldibenzo-18-crown-6( image 3 ), yield 54.6%, purity 65.2%.

Embodiment 3

[0028] a. Weigh 6.2g (0.05mol) of p-methylcatechol and 71.25g (0.25mol) of cesium carbonate and dissolve them in 400ml of tetrahydrofuran, wherein the cesium carbonate is added in two equal amounts. Weigh 0.085 mol of diethylene glycol xylene sulfonate and dissolve it in 250 ml of tetrahydrofuran in two equal amounts, and add dropwise in a constant pressure dropping funnel. The reaction was carried out at 50°C for 60 hours, and the reaction conversion rate was 49.5%.

[0029] b. filter the mixture obtained according to the above step a, weigh 5g of the mixture after distillation under reduced pressure, add 250g of thin-layer chromatography silica gel and 300ml of n-hexane, reflux and co-heat for 6h at 60°C, filter the filtrate, and vacuum distill the filtrate. Recrystallization gave 4', 5"-dimethyldibenzo-18-crown-6( Figure 4 ), yield 47.1%, purity 70.9%.

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Abstract

The invention discloses an extracting agent for nuclear waste liquid. The extracting agent is a compound of 4',4''(5'')-dimethyldibenzo-18-crown-6; one methyl in dimethyl is positioned at a 4' position of a benzene ring on one side; and the other methyl is positioned at a 4'' or 5'' position of a benzene ring on the opposite side. The compound has a function of extracting 137Cs+ ions from the nuclear waste liquid. A raw material, namely para-methyl pyrocatechol, for preparing the 4',4''(5'')-dimethyldibenzo-18-crown-6 is difficultly oxidized, byproducts generated in the reaction process of the 4',4''(5'')-dimethyldibenzo-18-crown-6 are reduced, a separation flow is simplified, and the yield is improved.

Description

technical field [0001] The invention relates to a nuclear waste liquid extractant and a preparation method thereof. Background technique [0002] The macrocyclic structure of the crown ether compound has specific selectivity for metal ions, especially for alkali metals and alkali metals, which have super selectivity and coordination ability. For example, dibenzo-18-crown 6 exhibits the effect on high-level radioactive waste liquid 137 The selective extraction function of Cs has made it one of the research hotspots of radioactive ion extractants in recent years. [0003] However, the polar structure of dibenzo-18-crown 6 leads to its low lipophilicity and poor solubility in non-polar solvents, which limit its application in the nuclear industry. The simultaneous introduction of alkyl side chains on the two benzene rings of dibenzo-18-crown 6 can increase its lipophilicity without changing its extraction ability, such as the commercially available 4', 4"(5")- Di-tert-butyl ...

Claims

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Application Information

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IPC IPC(8): C07D323/00C22B26/10
Inventor 杨伯伦范娟伊春海兰晓荣
Owner XI AN JIAOTONG UNIV
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