Use and method of amino-containing neutral phosphine extractant for extracting and separating tetravalent cerium
An extractant and neutral phosphine technology, which is applied in the application field of amino-containing neutral phosphine extractant in the separation of tetravalent cerium, can solve the problems of high extraction and separation cost, high price, difficult back extraction, etc., and achieve good extraction Separation ability, reduced extraction and separation cost, simple and easy access to chemical raw materials
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[0100] In order to further illustrate the solutions of the present invention, specific examples of the present invention are provided to help those skilled in the art understand and implement the present invention, but the present invention is not limited to these examples.
[0101] Reagents and sources
[0102] Diethylhexyl phosphite, di-n-octyl phosphite, di-n-heptyl phosphite, di-isooctyl phosphite, aviation kerosene and TBP were purchased from Shanghai Laish Chemical Co., Ltd.
[0103] Paraformaldehyde, di-n-hexylamine, diisobutylamine, n-butylamine, diisooctylamine, dodecylamine, isooctylamine, dimethylamine, toluene, xylene, p-toluenesulfonic acid, and heptane purchased from Aladdin Reagent Co., Ltd.
[0104] Cyanex 923 and 2-methylheptanol were purchased from Shanghai Cyanex Chemical Co., Ltd.
[0105] Feed liquid, washing liquid and stripping agent are self-made in the laboratory.
[0106] Other reagents (such as acids, etc.) are commercially available analytical re...
preparation example 1
[0109] Preparation Example 1: Preparation of (N,N-dihexylamino)methylphosphonic acid bis(2-ethylhexyl)ester
[0110]
[0111] In a three-necked flask equipped with a mechanical stirrer, a water separator, and a condensation reflux device, add diethylhexyl phosphite (1mol), paraformaldehyde (M=30, 1.05mol), di-n-hexylamine (1.05mol) , toluene (700ml) and p-toluenesulfonic acid (2g), heated to reflux at 130°C, and the water generated by the reaction was separated. When anhydrous is produced, react for another 2 hours. 10 g of potassium carbonate was added to the reaction mixture, and heating to reflux was continued for 15 min. The reaction mixture was filtered to remove excess potassium carbonate in the reaction, washed three times with distilled water, and the toluene was removed by rotary evaporation to obtain the target product.
[0112] 1 H NMR (400MHz, CDCl 3 ,ppm): δ1.74-0.86[m,(CH 3 ) 6 ,(CH 2 ) 16 ,(CH) 2 ],2.63[m,(CH 2 )],2.95[t,CH 2 , J=8Hz], 3.96[m, (CH ...
preparation example 2
[0113] Preparation Example 2: Preparation of Dioctyl (N,N-Diisobutylamino)methylphosphonate
[0114]
[0115] Except that di-n-octyl phosphite was used to replace diethylhexyl phosphite and diisobutylamine was used to replace di-n-hexylamine, the target product was prepared by the same process as in Preparation Example 1.
[0116] 1 H NMR (400MHz, CDCl 3 ,ppm): δ1.71-0.89[m,(CH 3 ) 6 ,(CH 2 ) 12 ],2.05[m,(CH) 2 ],2.31[m,(CH 2 ) 2 ],2.95[m,(CH 2 )],4.02[m,(CH 2 ) 2 ].
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