Anhydrous high-purity rare earth fluoride and preparation method thereof
A technology of rare earth fluoride and high water content, applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of long sedimentation and clarification time, high content of non-rare earth impurities, difficulty in filtration and washing, etc.
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Embodiment 1
[0023] Example 1 Anhydrous high-purity yttrium fluoride and its preparation
[0024] Preparation of high-purity yttrium chloride purification solution
[0025] REO concentration: 100-120g / l
[0026] Y purity: >99.999%
[0027] Fe 2 o 3 2 O<0.05mg / L
[0028] Free acidity: [H + ]≤0.50mol / L
[0029] Deionized water (DW)
[0030] Resistance > 12 megohms, total salinity 2 <70μg / l
[0031] Refined oxalic acid (H 2 C 2 O 4 ·2H 2 O)
[0032] Fe 2 o 3 2 <5ppm
[0033] Analytical grade hydrofluoric acid (HF)
[0034] Content (HF) > 40%
[0035] Fe 2 o 3 2 <5ppm
[0036] Chloride (Cl) <10ppm Phosphate <2ppm
[0037] Sulfates and sulfites (as SO 4 Count)<20ppm
[0038] 22% Reagent NH 4 Oh
[0039] Concentration (equivalent): 11.87mol / L
[0040] Fe 2 o 3 2 <5ppm
[0041] Ammonium bicarbonate solution
[0042] [OH - ] / [HCO 3 - ]=0.67-0.8
[0043] Fe 2 o 3 2 <5ppm
[0044] Compound fluorinating agent
[0045] Molar ratioHF / NH...
Embodiment 2
[0079] Example 2 Anhydrous high-purity lanthanum fluoride and its preparation
[0080] Preparation of Purification Solution of High Purity Lanthanum Chloride
[0081] REO concentration: 120-130g / l
[0082] La purity: >99.99%
[0083] Fe 2 o 3 2 O<0.05mg / L
[0084] Free acidity: [H + ]≤0.50mol / L
[0085] All the other conditions and operations are the same as in Example 1.
[0086] Anhydrous high-purity rare earth lanthanum fluoride quality index
[0087] project
unit
LaF 3
TREO
%
≥99.99
La 2 o 3 / TREO
ppm
≤10
CeO 2 / TREO
ppm
≤10
PR 6 o 11 / TREO
ppm
≤10
Nd 2 o 3 / TREO
ppm
≤10
SM 2 o 3 / TREO
ppm
≤10
Fe 2 o 3 / M
ppm
≤1
CaO / M
ppm
≤10
SiO 2 / M
ppm
≤10
Mn / M
ppm
≤1
Na / M
ppm
≤3
Pb / M
ppm
≤3
Zn / M
ppm
≤3
Al / ...
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