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Method for precipitation of low-chloride lutetium oxide by chloride system

A chloride and lutetium oxide technology, applied in chemical instruments and methods, rare earth metal compounds, inorganic chemistry, etc., can solve problems such as high impurities and chloride ion encapsulation, and achieve the effects of low impurities, easy industrialization, and large output.

Active Publication Date: 2019-10-25
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

[0005] The purpose of the present invention is to provide a method for precipitating low-chloride lutetium oxide in a chloride system, which can effectively prevent the problem of chloride ion encapsulation and the problem of high impurities caused by powder agglomeration during the precipitation of lutetium oxalate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0016] The invention discloses a method for precipitating lutetium oxide with a chloride system, 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 1.359...

Embodiment 2

[0024] (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.

[0025] (2) Precipitant preparation: use refined oxalic acid solution with a concentration of 120g / L, the volume of refined oxalic acid solution is 0.485m 3 , where Fe, Ca, SO 4 2- The mass ratio of t...

Embodiment 3

[0031] (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.

[0032] (2) Precipitant preparation: Use refined oxalic acid solution with a concentration of 150g / L, the volume of refined oxalic acid solution is 0.655m 3 , where Fe, Ca, SO 4 2- The mass ratio of the mass of impurities to the refined oxalic acid soluti...

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Abstract

The invention discloses a method for precipitation of low-chloride lutetium oxide by a chloride system. The method includes the following steps that (1) feed liquid preparation is conducted, specifically, a LuCl3 solution with the concentration being 0.1-0.8 mol / L and a concentrated nitric acid solution are mixed and stirred to form feed liquid with the stable concentration, and the nitrate concentration in the feed liquid is 0.3-2.0 mol / L; (2) precipitant preparation is conducted, specifically, an oxalic acid solution with the concentration being 120-150 g / L is used, and heated until solid oxalic acid in the oxalic acid solution is completely dissolved, and thus a precipitant is prepared; (3) chloride is removed by precipitation, specifically, a concurrent flow precipitation method is used for mixed reaction and precipitation of bottom water, the feed liquid, and the precipitant at a temperature of 35-60 DEG C, and the stoichiometric ratio of lutetium chloride and oxalic acid which are put in a reaction is n(the chloride lutetium ):n(the oxalic acid)=1: (1.65 to 1.95); (4) the chloride is removed by washing, specifically, a precipitant, namely a lutetium oxalate hydrate is washed;and (5) burning is conducted, specifically, the washed precipitant, namely the lutetium oxalate hydrate is burned to obtain a low-chloride lutetium oxide product so as to prevent high impurities caused by the inclusion of chloride ions and powder agglomeration in the precipitation process of the lutetium oxalate hydrate.

Description

technical field [0001] The invention belongs to the field of rare earth materials, relates to a method for precipitating low-chloride lutetium oxide in a chloride system, and 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 scintillati...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
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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