Method for separating tetravalent cerium, thorium and rare earth
A rare earth and solid-state separation technology, which is applied in the field of thorium and rare earth and tetravalent cerium separation, can solve the problem that the medium can only be nitric acid, etc., and achieve the effects of strong extraction ability, elimination of influence, shortening the separation process and cost
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[0142] Example
[0143] In order to further illustrate the solution of the present invention, specific embodiments 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 embodiments.
[0144] Reagents and sources
[0145] Diethylhexyl phosphite, di-n-octyl phosphite, di-n-heptyl phosphite, di-iso-octyl phosphite, aviation kerosene and TBP were purchased from Shanghai Laiyashi Chemical Co., Ltd.
[0146] Paraformaldehyde, di-n-hexylamine, diisobutylamine, n-butylamine, diisooctylamine, dodecylamine, isooctylamine, dimethylamine, toluene, xylene, p-toluenesulfonic acid and heptane Purchased from Aladdin Reagent Co., Ltd.
[0147] Cyanex923 and 2-methylheptanol were purchased from Shanghai Cytec Chemical Co., Ltd.
[0148] The material liquid, washing liquid and stripping agent are made by the laboratory.
[0149] Other reagents (such as acids, etc.) are commercially available a...
Example Embodiment
[0152] Preparation Example 1: Preparation of (N,N-Dihexylamino)Di(2-ethylhexyl)methylphosphonate
[0153]
[0154] Add diethylhexyl phosphite (1mol), paraformaldehyde (M=30, 1.05mol), and di-n-hexylamine (1.05mol) into a three-necked flask equipped with a mechanical stirrer, a water separator and a reflux device for condensation. , Toluene (700ml) and p-toluenesulfonic acid (2g), heated to reflux at 130°C to separate the water produced by the reaction. When no water is generated, react for another 2 hours. 10 g of potassium carbonate was added to the reaction mixture, and heating and refluxing were continued for 15 min. The reaction mixture was filtered to remove excess potassium carbonate in the reaction, washed with distilled water three times, and the toluene was removed by rotary evaporation to obtain the target product.
[0155] 1 HNMR(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 2 ) 2 ].
Example Embodiment
[0156] Preparation Example 2: Preparation of dioctyl (N,N-diisobutylamino)methylphosphonate
[0157]
[0158] Except that di-n-octyl phosphite was used instead of diethylhexyl phosphite and diisobutylamine was used instead of di-n-hexylamine, the target product was prepared by the same process as in Preparation Example 1.
[0159] 1 HNMR(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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