Preparation and use of hydroxyl oximated calix[6]arene efficient uranium extractant

A technology for hydroximating calixarene derivatives, which is applied in the field of synthesis of calixarene derivatives, can solve the problems of cumbersome synthesis routes, harsh reaction conditions, and many reaction parameters of calixarene hydroxime derivatives, and achieve high extraction performance and selectivity The effect of bit performance, short reaction time, and simple synthesis route

Inactive Publication Date: 2013-08-14
NANHUA UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to the published literature reports, the synthetic routes of calixarene hydroxime derivatives are either complicated, or the reaction time is long and the reaction conditions are harsh.
For example, the synthesis method of calixarene-hydroxamic acid disclosed in Document 1 (Sichuan University 2003 master's degree thesis "Design and Synthesis of Calixarene-Hydroxamic Acid and the Enzyme-like Function of Transition Metal Complexes") uses four One-step or five-step synthet

Method used

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  • Preparation and use of hydroxyl oximated calix[6]arene efficient uranium extractant
  • Preparation and use of hydroxyl oximated calix[6]arene efficient uranium extractant
  • Preparation and use of hydroxyl oximated calix[6]arene efficient uranium extractant

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] First, the phenolic hydroxyl group of calix [6] arene is converted into an ester group, and the ethyl acetate derivative of calix [6] arene is obtained, and the molecular formula is C 90 h 120 o 18 , the structural formula is as follows:

[0019]

[0020] Then, using calix[6]arene ethyl acetate derivatives as raw materials, the ester group is directly converted into a hydroxime group by reacting with hydroxylamine hydrochloride to obtain a hydroximated calix[6]arene with the molecular formula C 78 h 102 o 18 N 6 , the structural formula is as follows:

[0021]

[0022] The method of the present invention achieves the purpose of reducing the synthesis cost and improving the yield by simplifying the synthesis route and improving the reaction conditions. The synthesis route is as follows:

[0023]

[0024]

[0025] Specific steps are as follows:

[0026] The first step, the preparation of calix[6]arene ethyl acetate derivatives: Weigh 3.605g calix[6]aren...

Embodiment 2

[0029] Take 100mL of uranium solution of 5mg / L-10mg / L, adjust the pH value between 4.0-7.0, weigh 0.0509g of the hydroximated calix[6]arene prepared in Example 1 and dissolve it in 100mL of chloroform solution, carry out In the liquid-liquid extraction experiment, after 20 minutes, the supernatant of the raffinate phase was taken by standing for stratification, and the residual uranium concentration was measured by spectrophotometry. The results showed that the extraction rate of uranium by hydroximated calix[6]arene reached 99% above.

Embodiment 3

[0031] With reference to the content of alkali metals and alkaline earth metals in seawater, prepare 1% Na + , 1%K + , 1‰Ca 2+ and 1‰Mg 2+ The aqueous solution that coexists with the uranium of 5mg / L, carries out extraction test by the method in embodiment 2, adopts spectrophotometry to measure the residual uranium concentration of raffinate phase, and the result shows that under the coexistence condition of alkali metal and alkaline earth metal, hydroximation cup [6] The extraction rate of uranium by aromatics is over 98%.

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Abstract

The invention discloses a synthetic method of hydroxyl oximated calix[6]arene suitable for efficient uranium extraction. The synthetic method is completed by two steps: firstly, performing reaction between calix[6]arene and ethyl bromoacetate under the catalytic effect of anhydrous potassium carbonate to obtain a calix[6]arene ethyl acetate derivative; and secondly, performing reaction between the calix[6]arene ethyl acetate derivative and hydroxylamine hydrochloride under the catalytic effect of potassium hydroxide to obtain hydroxyl oximated calix[6]arene. The method is simple and convenient in synthetic line, mild in reaction condition and easy to control and realize; and synthesized hydroxyl oximated calix[6]arene has efficient extraction performance and selective complexation performance to uranium and has wide application prospect in uranium separation, uranium-bearing wastewater treatment and uranium recovery.

Description

technical field [0001] The invention belongs to the field of organic oligomer materials, and in particular relates to the synthesis of calixarene derivatives suitable for high-efficiency extraction of uranium. Background technique [0002] With the rapid development of nuclear power in my country, the demand for uranium is increasing year by year. At present, the domestic production capacity of natural uranium can only meet 1 / 3 of the demand, and the supply of uranium is under great pressure. However, a large amount of waste liquid produced by uranium mining and metallurgy and low content of uranium in waste water pose a threat to the ecological environment, and the existing treatment technology cannot fully recover uranium in such waste water and waste liquid. In order to improve the utilization rate of uranium resources, ensure the uranium supply for nuclear power development, promote the clean production and environmental protection of uranium mining and metallurgy, it is...

Claims

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Application Information

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IPC IPC(8): C07C239/14C22B60/02C22B3/26
Inventor 王劲松方丰荣谢水波刘迎九周洁皮艾南莫辉艳
Owner NANHUA UNIV
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