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Anhydrous high-purity rare earth fluoride and preparation method thereof
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A rare earth fluoride, high water technology, applied in rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., can solve the problems of difficult filtration and washing, long precipitation and clarification time, and high content of non-rare earth impurities
Active Publication Date: 2010-08-18
QIANDONG RARE EARTH GRP
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At present, most manufacturers adopt the wet method. Although the conventional wet method is easy to operate, the precipitated rare earth fluoride is in the form of colloid, which is difficult to filter and wash. It takes a long time to clarify the precipitate, especially the high content of non-rare earth impurities, so it cannot be used directly. In the field of electronics and luminescent materials, it is necessary to provide anhydrous high-purity rare earth fluorides and their preparation methods
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Embodiment 1
[0023] Example 1 Anhydrous high-purity yttrium fluoride and its preparation
[0024] Preparation of high-purity yttriumchloride 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
[0080] Example 2 Anhydrous high-purity lanthanum fluoride and its preparation
[0081] Preparation of Purification Solution of High Purity LanthanumChloride
[0082] REO concentration: 120-130g / l
[0083] La purity: >99.99%
[0084] Fe 2 o 3 2 O<0.05mg / L
[0085] Free acidity: [H + ]≤0.50mol / L
[0086] All the other conditions and operations are the same as in Example 1.
[0087] Anhydrous high-purity rare earth lanthanum fluoride quality index
[0088] 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 / M
ppm
...
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Abstract
The invention discloses an anhydrous high-purity rare earthfluoride and a preparation method thereof. The anhydrous high-purity rare earthfluoride mainly comprises minim non-rare earthimpurity iron (Fe2O3<=1ppm), calcium (CaO<=10ppm), silicon (SiO2<=10ppm), carbon (C<=200ppm), oxygen (O<=200ppm), chloride (Cl<=30ppm), sulfur (S<=10ppm) and the like and has ignition loss not more than 0.5%. The product is mainly applied in the field of electronic and luminescent materials. The preparation method is characterized by pre-removing the non-rare earth impurity by enhancement on the basis of the traditional process and then carrying out conversion in the form of compound fluorinating agents; strictly controlling the feed liquor concentration and acidity, fluorinating agent addition, fluorination temperature and time, etc and obtaining the rare-earth fluoride which is coarse in fluorinated particles, fast in sedimentation and easy to wash and filter; and finally obtaining the anhydrous high-purity rare earth fluoride product through subsequent drying and particle integration.
Description
technical field [0001] The invention belongs to the technical field of solventprecipitation conversion synthesis of rare earth salts, in particular to anhydrous high-purity rare earth fluorides and a preparation method thereof. Background technique [0002] In the early days, rare earth fluorides were mainly used as luminescent agents for arc carbon rods to fill the center of anode carbon rods; in addition, as additives for steel and non-ferrous alloys, they played the role of desulfurization and deoxidation; It is a fluoride systemelectrolysis used as a molten salt, which forms a molten saltelectrolyte with lithium fluoride and barium fluoride to prepare rare earth metals, and is also used as a raw material for the preparation of a single rare earth metal by metallothermal reduction; with the development of science and technology, in recent years The use of rare earth fluorides in the fields of electronic materials, polishing materials and conversion luminescent material...
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