Technology for recovery of uranium in ceramic UO2 pellet by supercritical CO2 extraction
A supercritical and extraction technology, which is applied in the field of uranium in ceramic UO2 pellets extracted by supercritical CO2, can solve the problems of small ion exchange treatment capacity, large critical safety hazards, and low degree of automation, so as to reduce critical safety hazards, High extraction efficiency and selectivity, high degree of automation
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Embodiment 1
[0023] 1. Sc-CO 2 / TBP-HNO 3 Preparation: use 60% ~ 70% HNO 3 Mix-clarify operation with TBP, adjust HNO by adding TBP 3 / TBP ratios are 0.6, 0.8, 1.0, 1.3, 1.4, and finally used as the extraction agent used in the process, and then it is placed in a closed container, and CO 2 , adjust the temperature at 50°C to 60°C; the pressure at 10MPa, stabilize the system until a uniform Sc-CO 2 / TBP-HNO 3 supercritical phase.
[0024] 2. Extraction sample preparation: the ceramic UO 2 The pellets are placed in a calciner, fed with air or oxygen, and calcined at 850°C to 900°C for 4h to 5h.
[0025] 3. Extraction and separation of the first group: different HNO as described in step 1 3 / TBP ratio, the extraction was carried out under the conditions of temperature 60°C, pressure 15MPa, extraction time 2h, extraction agent 30mL, and extraction sample 7g. After the extraction is completed, the loaded supercritical phase is transferred to the separator for separation.
[0026] 4. Se...
Embodiment 2
[0029] 1. Carry out Sc-CO according to the requirements of 1 and 2 in Example 1 2 / TBP-HNO 3 Preparation and Extraction Sample Preparation.
[0030] 2. Extractant usage control: control Sc-CO 2 / TBP-HNO 3 Medium TBP-HNO 3 The organic phases were 20mL, 25mL, 27mL, 30mL, 40mL, respectively.
[0031] 3. Extraction and separation of the second group: In step 2, the amount of different extractants used, respectively at a temperature of 60°C, a pressure of 15MPa, an extraction time of 2h, and HNO 3 / TBP ratio of 1.4, the extraction sample was extracted under the conditions of 7g. After the extraction is completed, the loaded supercritical phase is transferred to the separator for separation.
[0032] 4. Separation of the extraction product is carried out according to the requirements of step 4 in Example 1. After complete separation, the product was collected.
[0033] As the amount of extractant used increases, the extraction efficiency of uranium increases linearly until t...
Embodiment 3
[0035] 1. Carry out Sc-CO according to the requirements of 1 and 2 in Example 1 2 / TBP-HNO 3 Preparation and Extraction Sample Preparation.
[0036] 2. Extraction and separation of the third group: at a temperature of 60°C, a pressure of 15MPa, an extractant of 30mL, HNO 3 Under the conditions of / TBP ratio 1.4 and extraction sample 7g, the six groups of samples were extracted for 15min, 30min, 45min, 60min, 90min, 120min respectively. After the extraction is completed, the loaded supercritical phase is transferred to the separator for separation.
[0037] 3. Separation of the extraction product is carried out according to the requirements of step 4 in Example 1. After complete separation, the product was collected for analysis.
[0038] With the increase of extraction time, the extraction efficiency of uranium increased slowly at first, then accelerated after 30 minutes, and the complete extraction of uranium could be basically realized after 45 minutes.
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