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Preparation method of lanthanum-cerium hydroxides with high oxidation rate

A hydroxide, oxidation rate technology, applied in rare earth metal oxides/hydroxides, chemical instruments and methods, rare earth metal compounds, etc. Efficiency, low content of non-rare earth impurities, effect of reducing the introduction of non-rare earth impurities

Active Publication Date: 2016-08-03
YIYANG HONGYUAN RARE EARTH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is to provide a method for preparing lanthanum cerium hydroxide with a high oxidation rate in view of the insufficient oxidation rate of the existing lanthanum cerium hydroxide element

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Cerium carbonate (CeO 2 ≥99.995wt%) and lanthanum carbonate (La 2 o 3 ≥99.99wt%) are dissolved with nitric acid respectively, the addition of nitric acid is controlled, the pH is adjusted back to 4.5 with cerium carbonate or lanthanum carbonate respectively, and 15wt% (NH 4 ) 2 S reagent, the amount of reagent added is 0.05% of the volume of the feed liquid, let it stand for 15 hours, filter it three times with a filter cloth to obtain the filtrate, then add deionized water to the filtrate to dilute until the concentration of the filtrate is 40g / L, and store it statically. stand-by;

[0022] Take 1L of the diluted cerium nitrate feed solution and add 25mL of oxidizing agent (50% hydrogen peroxide), stir for 5min, then add 10mL of 5mol / L ammonia water, adjust the pH to ≥ 5.0, and stir for 5min;

[0023] Add 0.5 liter of 40g / L lanthanum nitrate feed solution, heat to 30°C, add 25 mL of oxidant (50% hydrogen peroxide) again, stir, add 100 mL of 10 mol / L ammonia water, ...

Embodiment 2

[0027] Cerium carbonate (CeO 2 ≥99.99wt%) and lanthanum carbonate (La 2 o 3 ≥99.99wt%) are dissolved with nitric acid respectively, the addition of nitric acid is controlled, the pH is adjusted back to 4.0 with cerium carbonate or lanthanum carbonate respectively, and 12wt% (NH 4 ) 2 S reagent, the amount of reagent added is 0.08% of the volume of the feed liquid, let it stand for 20 hours, filter it twice with a filter cloth, and obtain the filtrate, then add deionized water to the filtrate to dilute until the concentration of the filtrate is 50g / L, and store it standing still ,stand-by;

[0028] Take 1L of the diluted cerium nitrate feed solution and add 35mL of oxidizing agent (50% hydrogen peroxide), stir for 5min, then add 25mL of 1mol / L ammonia water, adjust the pH to ≥ 5.0, and stir for 5min;

[0029] Add 0.4 liter of 50g / L lanthanum nitrate feed solution, heat to 35°C, add 45mL of oxidizing agent (50% hydrogen peroxide) again, stir, add 150mL of 5mol / L ammonia wate...

Embodiment 3

[0033] Cerium carbonate (CeO 2 ≥99.995wt%) and lanthanum carbonate (La 2 o 3 ≥99.99wt%) are dissolved with nitric acid respectively, the addition of nitric acid is controlled, the pH is adjusted back to 4.8 with cerium carbonate or lanthanum carbonate respectively, and 16wt% (NH 4 ) 2 S reagent, the amount of reagent added is 0.2% of the volume of the feed liquid, let it stand for 25 hours, filter it four times with a filter cloth to get the filtrate, then add deionized water to the filtrate to dilute until the concentration of the filtrate is 30g / L, and store it standing still ,stand-by;

[0034] Take 1L of diluted cerium nitrate feed solution and add 20mL of oxidizing agent (50% hydrogen peroxide), stir for 10min, then add 15mL of 2mol / L ammonia water, adjust the pH to ≥ 5.0, and stir for 5min;

[0035] Add 0.5 liter of 30g / L lanthanum nitrate feed solution, heat to 40°C, add 30mL of oxidant (50% hydrogen peroxide) again, stir, add 70mL of 15mol / L ammonia water, and adju...

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Abstract

The invention discloses a preparation method of lanthanum-cerium hydroxides with a high oxidation rate. The preparation method comprises the following steps: (1) individually dissolving cerium carbonate and lanthanum carbonate by nitric acid, controlling the addition amount of nitric acid, and adjusting the pH value until the pH value is not less than 4.0 by carbonates, adding a (NH4)2S reagent, allowing the systems to stand still for 15 to 30 hours, filtering the solutions for 2 to 5 times, and diluting the filtrates by deionized water; (2) adding an oxidant into the cerium nitrate solution, stirring, and adjusting the pH value until the pH value is not less than 5.0 by ammonia water; (3) adding lanthanum nitrate solution, heating to a temperature of 25 to 40 DEG C, adding an oxidant, stirring, and adjusting the pH value until the pH value is more than 9 by ammonia water; (4) heating to a temperature of 55 to 65 DEG C, stirring at a constant temperature, heating to a temperature of 90 to 105 DEG C to carry out decomposition, stirring at a constant temperature, allowing the solution to stand still to clarify the solution, performing press filtration, washing, and drying. The TREO of obtained product is more than 70%, the oxidation rate of Ce is more than 99.9%, the solution is clear, the non-rare earth impurity content is low, the NaO content is not more than 5 ppm, the NH4<+> content is not more than 0.1%, and the NO3<-> content is not more than 2.0%.

Description

technical field [0001] The invention belongs to the production technology of rare earth compounds in the field of hydrometallurgy, and in particular relates to a preparation method of lanthanum cerium hydroxide with high oxidation rate. Background technique [0002] With the development of science and technology, the status of rare earth products in the national economy is becoming more and more important, and the output of light rare earths accounts for 80% of rare earth products. Light rare earths are mainly used in preservatives, laboratory reagents, organic intermediates, The demand for fine chemicals, catalytic additives, biopharmaceuticals, automobile exhaust purifiers, petroleum catalytic cracking, etc. is increasing, and the requirements for the physical and chemical properties of products are also getting higher and higher. [0003] At present, the production of lanthanum hydroxide cerium generally adopts the traditional cerium hydroxide precipitation method, such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01F17/00
CPCC01F17/206
Inventor 崔小震肖勇曾志平郭卫权陈月华刘卫任萍许鸽明朱焱
Owner YIYANG HONGYUAN RARE EARTH
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