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A method for preparing low-chloride lutetium oxide

A technology of lutetium oxide and chloride, applied in chemical instruments and methods, lanthanum oxide/lanthanum hydroxide, lanthanide oxide/hydroxide, etc., can solve the problem of cost increase, product yield reduction, chloride wrapping, etc. problems, to achieve the effect of simple process control, low product impurities, and simplified process

Active Publication Date: 2020-05-29
FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The impact of impurity ions in lutetium oxide products on crystal performance is also particularly important. According to relevant literature reports, impurity ions will directly affect the light output of rare earth scintillation crystals LSO or LYSO, and affect the efficiency of PET testing. The main impurity ions in lutetium oxide are Chloride ions, chloride ions have negative 1 valence, while oxygen ions in rare earth scintillation crystals LSO or LYSO have negative 2 valences. When lutetium oxide is used to make scintillation crystals, chloride ions will replace oxygen ions, causing crystal defects and affecting crystal performance.
[0004] At present, the content of chloride radicals in lutetium oxide prepared by precipitation method is about 100~200ug / g, and the situation of chloride radical encapsulation is very easy to occur during the precipitation process of lutetium oxide, resulting in high chloride radicals in lutetium oxide after burning
However, the use of lutetium oxide for secondary precipitation through nitric acid redissolution will lead to problems such as reduced product yield and increased cost.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The invention discloses a method for preparing low-chloride lutetium oxide, comprising the following steps:

[0017] (1) Material liquid preparation: concentration is 0.5mol / L and volume is 0.5m 3 LuCl 3 solution, add 2m 3 Add 51.7L of concentrated nitric acid solution with a concentration of 65%~68% to the container, mix and stir until a feed liquid with a stable concentration is formed, that is, after mixing for 1 hour, detect the concentration of lutetium chloride in the feed liquid, and the concentration of lutetium chloride The deviation of the calculated value of the concentration is no more than 0.02mol / L, which is to form a stable concentration of feed liquid. In the present embodiment, the calculated value of the concentration of lutetium chloride is 0.437mol / L. After stirring for 1h, the concentration of the detection solution is 0.417~0.457mol / L, it is judged to be uniformly mixed. Wherein the nitrate concentration in the feed liquid is 1.359mol / L, n(Lu 3...

Embodiment 2

[0025] The invention discloses a method for preparing low-chloride lutetium oxide, comprising the following steps:

[0026] (1) Material liquid preparation: concentration is 0.35mol / L and volume is 0.8m 3 LuCl 3 solution, add 2m 3 Add 57.9L of concentrated nitric acid solution with a concentration of 65%~68% to the container, mix and stir until a feed liquid with a stable concentration is formed, that is, after mixing for 1 hour, detect the concentration of lutetium chloride in the feed liquid, and the concentration of lutetium chloride The deviation of the calculated value of the concentration is not more than 0.02mol / L, and then a feed liquid with a stable concentration is formed. Wherein the nitrate concentration in the feed liquid is 0.978mol / L, n(Lu 3+ ):n (NO 3 - )=1:3, where, n(Lu 3+ )=0.35mol / L*800L=280mol, n(NO 3 - )=14.5mol / L *57.9L=840mol, so n(Lu 3+ ):n (NO 3 - )=1:3.

[0027] (2) Precipitant preparation: use refined oxalic acid solution with a concentr...

Embodiment 3

[0034] The invention discloses a method for preparing low-chloride lutetium oxide, comprising the following steps:

[0035] (1) Material liquid preparation: concentration is 0.8mol / L and volume is 0.5m 3 LuCl 3 solution, add 2m 3 Add 82.75L of concentrated nitric acid solution with a concentration of 65%~68% to the container, mix and stir until a feed liquid with a stable concentration is formed, that is, after mixing for 1 hour, detect the concentration of lutetium chloride in the feed liquid, and the deviation from the calculated value is the same. If it exceeds 0.02mol / L, it will form a feed liquid with a stable concentration. Wherein the nitrate concentration in the feed liquid is 2.0mol / L, n(Lu 3+ ):n (NO 3 - )=1:3, where, n(Lu 3+ )=0.8mol / L*500L=400mol, n(NO 3 - )=14.5mol / L *82.75L=1200mol, so n(Lu 3+ ):n (NO 3 - )=1:3.

[0036] (2) Precipitant preparation: Use refined oxalic acid solution with a concentration of 150g / L, the volume of refined oxalic acid solu...

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PUM

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Abstract

The invention discloses a method for preparing low-chloride lutetium oxide, which comprises the following steps: (1) Preparation of feed liquid: LuCl with a concentration of 0.1-0.8 mol / L 3 The solution is mixed with the concentrated nitric acid solution to form a feed liquid with a stable concentration. The concentration of nitrate in the feed liquid is 0.3~2.0mol / L; (2) Precipitant preparation: use oxalic acid solution with a concentration of 120~150g / L, Completely dissolve the solid oxalic acid in the oxalic acid solution to make a precipitant; (3) Chlorine removal by precipitation: use the co-current precipitation method to mix the bottom water, the above-mentioned feed liquid and the above-mentioned precipitant at a temperature of 35~60°C to react and precipitate , so that the stoichiometric ratio of lutetium chloride and oxalic acid input into the reaction is n(lutetium chloride):n(oxalic acid)=1: (1.65~1.95); (4) washing and removing chlorine radicals: washing the precipitate lutetium oxalate ; (5) Burning: burn the washed precipitate lutetium oxalate to obtain low-chloride lutetium oxide products to prevent chloride ion wrapping and powder agglomeration during the precipitation of lutetium oxalate, resulting in high impurities.

Description

technical field [0001] The invention belongs to the field of rare earth materials, and relates to a method for preparing low-chloride lutetium oxide, which is a preparation method of rare earth oxides. Background technique [0002] Positron Emission Computed Tomography (PET) system is widely used in the diagnosis and differential diagnosis of various diseases, disease judgment, curative effect evaluation, organ function research and new drug development, etc. In the PET system, background events caused by spontaneous emission of scintillation crystals, unreal random coincidence events and background noise caused by scattered coincidence events may have a great impact on the image signal-to-noise ratio. Therefore, the PET system usually adopts the following methods to ensure the signal-to-noise ratio of the image: reducing spontaneous emission and improving the energy resolution of the system. Among these methods, improving the quality index of scintillation crystal is a way...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/229
CPCC01P2006/80C01F17/271
Inventor 叶纪龙钟可祥张榕贵李来超
Owner FUJIAN CHANGJIANG GOLDEN DRAGON RARE EARTH CO LTD
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