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A kind of preparation method of high oxidation rate lanthanum cerium hydroxide

A hydroxide, oxidation rate technology, applied in rare earth metal oxides/hydroxides, chemical instruments and methods, rare earth metal compounds, etc. The effect of low impurity content

Active Publication Date: 2017-04-19
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%) were dissolved in nitric acid respectively, the amount of nitric acid added was controlled, the pH was adjusted to 4.5 with cerium carbonate or lanthanum carbonate respectively, and 15wt% (NH3) was added. 4 ) 2 Reagent S, the amount of reagent added is 0.05% of the volume of the feed solution, left for 15 hours, filtered with filter cloth three times to obtain a filtrate, and then added to the filtrate to dilute with deionized water until the concentration of the filtrate is 40g / L, and stored at rest, stand-by;

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

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

Embodiment 2

[0027] Cerium carbonate (CeO 2 ≥99.99wt%) and lanthanum carbonate (La 2 O 3 ≥99.99wt%) were dissolved in nitric acid respectively, the amount of nitric acid added was controlled, the pH was adjusted to 4.0 with cerium carbonate or lanthanum carbonate respectively, and 12wt% (NH3) was added. 4 ) 2 Reagent S, the amount of reagent added is 0.08% of the volume of the feed solution, left to stand for 20 hours, filtered twice with a filter cloth to obtain a filtrate, and then added deionized water to the filtrate to dilute to a filtrate concentration of 50g / L, and stored at rest ,stand-by;

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

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

Embodiment 3

[0033] Cerium carbonate (CeO 2 ≥99.995wt%) and lanthanum carbonate (La 2 O 3 ≥99.99wt%) were dissolved in nitric acid, the amount of nitric acid added was controlled, the pH was adjusted to 4.8 with cerium carbonate or lanthanum carbonate respectively, and 16wt% (NH3) was added. 4 ) 2 Reagent S, the amount of reagent added is 0.2% of the volume of the feed solution, left standing for 25 hours, filtered with filter cloth for four times to obtain a filtrate, and then added to the filtrate to dilute with deionized water until the concentration of the filtrate is 30g / L, and stored at rest ,stand-by;

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

[0035] Add 0.5 liter of 30g / L lanthanum nitrate feed solution, heat to 40°C, add 30 mL of oxidant (mass fraction is 50% hydrogen peroxide) again, stir, add ...

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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 rare earth compound production technology in the field of hydrometallurgy, and particularly 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 production of light rare earth accounts for 80% of rare earth products. Light rare earth is mainly used in preservatives, laboratory reagents, organic intermediates, The demand for fine chemicals, catalytic additives, biopharmaceuticals, automobile exhaust purifiers, and petroleum catalytic cracking is increasing, and the requirements for the physical and chemical properties of products are also getting higher and higher. [0003] At present, the traditional cerium hydroxide precipitation method is generally adopted in the production of lanthanum hydroxide, such as the ...

Claims

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Application Information

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Patent Type & Authority Patents(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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