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A method for recovering rare earth elements in waste red fluorescent powder

A technology of red fluorescent powder and rare earth elements, which is applied in the fields of rare earth metal compounds, chemical instruments and methods, inorganic chemistry, etc., and can solve problems that do not involve the recovery of rare earths

Active Publication Date: 2016-01-20
JIANGXI HUAKE RARE EARTH NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The law also does not involve the recovery of rare earths in color TV red phosphors and other red phosphors

Method used

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  • A method for recovering rare earth elements in waste red fluorescent powder

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Take 1000g of waste red phosphor powder for trichromatic fluorescent lamps, total rare earth (TREO): 81.56%, Eu 2 o 3 / TREO:7.25%, Y 2 o 3 / TREO: 92.73%, other rare earth 2 o 2 )(3%)-glacial acetic acid (CH 3 COOH) (8%), amount of rare earth metal: complex acid volume=1:3, acid-dissolution conditions are: acidity 0.5N, acid-dissolution temperature 90°C, after acid-dissolution, filter and remove insoluble matter to obtain 2.4L with a concentration of 338.1g / l The rare earth chloride solution, calculated rare earth dissolution yield is 99.5%. Dilute the rare earth chloride solution to a concentration of 120±5g / l and adjust the pH to 2.5±0.3, and enter the fractionated extraction system where the organic phase saponified with NaOH is 22% naphthenic acid+18% mixed alcohol+60% sulfonated kerosene Carry out extraction and separation, after 75 stages of extraction and 15 stages of washing, high-purity yttrium chloride (YCl 3 ) solution, the solution is precipitated and f...

Embodiment 2

[0019] Take 1000g of waste red phosphor powder for tricolor fluorescent lamps, total rare earth (TREO): 81.56%, EU 2 o 3 / TREO:7.25%, Y 2 o 3 / TREO: 92.73%, other rare earth 2 o 2 )(5%)-glacial acetic acid (CH 3 COOH) (3%), amount of rare earth metal: complex acid volume = 1: 3, acid-dissolution conditions are: acidity 0.5N, acid-dissolution temperature 110°C, after acid-dissolution, filter and remove insoluble matter to obtain 2.41L with a concentration of 337.0g / l The rare earth chloride solution, calculated rare earth dissolution yield is 99.6%. Subsequent processing steps are the same as in Example 1.

Embodiment 3

[0021] Take 1000g of waste red phosphor powder for trichromatic fluorescent lamps, total rare earth (TREO): 81.56%, Eu 2 o 3 / TREO:7.25%, Y 2 o 3 / TREO: 92.73%, other rare earth 3 )(89%)-Oxidizing agent (H 2 o 2 )(3%)-glacial acetic acid (CH 3COOH) (8%), amount of rare earth metal: complex acid volume=1:3, acid-dissolution conditions are: acidity 0.5N, acid-dissolution temperature 90°C, after acid-dissolution, filter and remove insoluble matter to obtain 2.41L with a concentration of 337.0g / l Rare earth nitrate solution, calculated rare earth dissolution yield is 99.6%. Dilute the rare earth nitrate solution to a concentration of 120±5g / l and adjust the pH to 2.5±0.3, then enter the fractionation extraction system where the organic phase saponified with NaOH is 22% naphthenic acid+18% mixed alcohol+60% sulfonated kerosene Extraction and separation, after 75 stages of extraction and 15 stages of washing, high-purity yttrium nitrate (Y(NO 3 ) 3 ) solution, the solution i...

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Abstract

The invention relates to a method for recovering rare earth elements from waste red phosphor. The method is characterized by: carrying out a calcination pretreatment on collected waste red phosphor in a calcination furnace kiln, and removing organic substances and other elements easily forming volatile gases in the red phosphor; carrying out dissolution decomposition on the calcined red phosphor in an acid (HCl, HNO3)-oxidant (H2O2)-stabilizing additive (acetic acid) composite acid system, and controlling to obtain a low acidity, such that rare earth elements such as Y and Eu or other rare earth in the red phosphor are preferentially dissolved, and completely enter the solution, and the other elements are insoluble substances, and are removed by filtration; after obtaining a rare earth acid solution, adopting an ammonia-free saponified fractionation extraction system to carry out extraction separation to obtain a high purity single rare earth chloride such as YCl3 and EuCl3 or other chlorinated rare earth enriched product solutions; and carrying out processes of precipitation and ignition to obtain a single rare earth oxide such as Y2O3 and Eu2O3 or other rare earth enriched product oxide products.

Description

technical field [0001] The invention relates to a method for comprehensive recycling of three wastes, in particular to a method for recycling rare earth elements in waste red fluorescent powder. Background technique [0002] According to statistics, the output of rare earth phosphors in my country reached 9,398 physical tons in 2010, an increase of 29.9% over the previous year. Among them, 8,000 tons of three-color phosphors for lamps (an increase of 33.3% over the previous year), 500 tons of color TV phosphors, 450 tons of long-lasting phosphors, and about 448 tons of other phosphors. It is estimated that by 2012, the output of rare earth phosphors in my country will reach 14,000 tons, and 6,500 tons of various rare earths will be consumed. In the production of phosphors, the production and replacement of tricolor fluorescent lamps, and the production and replacement of color TVs, a huge amount of phosphor waste is generated. It is estimated that by 2012, the waste of rare...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01F17/00
Inventor 廖爱阳
Owner JIANGXI HUAKE RARE EARTH NEW MATERIALS