Method for enriching and recovering extremely low concentration southern ionic rare earth by cellulose phosphate
A cellulose phosphate, ionic rare earth technology, applied in the direction of improving process efficiency, can solve the problem of incomplete separation of rare earth metals, etc., achieve good extraction effect, reduce entrainment problems, and reduce phosphorus loss.
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Embodiment 1
[0025] According to the ratio of mass:volume (kg / L) ratio of 1:20, dry cellulose was added to the pyridine solution; according to the ratio of mass:volume (kg / L) of 3:10, phosphorus trichloride Soluble in dichloromethane.
[0026] Slowly drop the above phosphorus trichloride mixture into the cellulose-containing pyridine solution, heat and reflux for 12 hours after the titration is completed, and pour the reaction solution into ice water after the reaction stops. The mixed solution was suction-filtered to obtain a solid, and the filter cake was washed with water and 0.1 mol / L hydrochloric acid, and air-dried to obtain phosphocellulose. The phosphorus content was determined to be 4.55%.
Embodiment 2
[0028] 25mL of ditch water (ditch water composition as follows: La, 5.36; Ce, 2.44; Nd, 4.85; Gd, 2.03; Dy, 3.49; Er: 2.30; Y: 20.89; Fe: 6.31; Al, 15.54; Si, 6.28; Mg, 11.33; Mn, 3.17; Na, 7.40; K, 28.39; Pd, 2.20 ug / mL) were added to 50 mg of the prepared phosphocellulose. Stir vigorously at room temperature for 2h.
[0029] The extract is separated from the phosphocellulose and the extract mother liquor by high-speed centrifugation. The concentration of each component in the rare earth ditch water was measured by ICP of the mother liquor, and it was found that the concentration of rare earth in the ditch water did not change much. while Fe 3+ with Al 3+ The concentrations were 0.16 ug / mL and 3.29 ug / mL. It shows that phosphoric acid fiber is greatly disturbed by Fe, Al ions and solution acidity when extracting ditch water.
Embodiment 3
[0031] Slowly drop 50 mL of ditch water with a pH value of 3.2 into aqueous ammonia to adjust the pH values to 4.0, 4.5, 5.2, and 5.6. White flocs appeared in the solution. Filter to remove flocs. The metal ion components in the filtrate were measured by ICP, and the total concentration of each rare earth metal was 42.2, 42.8, 39.0, 36.0 (ug / mL), indicating that under these pH conditions, the loss of rare earth metals in the stock solution is relatively small, while Fe and Al ions The loss is relatively large when the pH is 5.2 and 5.6. Respectively from 1.3 ug / mL to 0.07 ug / mL and 10.0 ug / mL to 2.1 ug / mL.
[0032] Measure 25 mL of the filtrate, add 50 mg of phosphocellulose, and stir vigorously at room temperature for 2 h.
[0033] The extract is separated from the phosphocellulose and the extract mother liquor by high-speed centrifugation. The concentration of each component of metal ions in the mother liquor was determined by ICP. It was found that when the pH value ...
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