Method for separating and recovering scandium in stable zirconia ceramic wastes containing scandium and rare earth

A technology of separation and recovery of zirconia ceramics, applied in the direction of improving process efficiency, etc., can solve the problems of low purity of recovered products, distribution and precipitation, large energy consumption, etc., and achieve high industrial use value, low recycling cost, and less waste water discharge Effect

Active Publication Date: 2015-05-27
HUNAN ORIENTAL SCANDIUM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] At present, the domestic method of recovering rare earth zirconium from waste zirconium ceramic materials containing rare earth mainly adopts alkali fusion method, such as CN201410205377.0, CN201210143905.5, CN200810073501.7 , patent, through two-stage eutectic sintering, then washed with water, acid-dissolved, high-temperature reaction in the process, large energy consumption, distributed precipitation, incomplete separation of zirconium and rare earth, and low purity of recovered products
In CN201310494964.1, hydrochloric acid + sulfuric acid + borate is used for dissolution. Although there is recovery of scandium, the process is dissolved at a high temperature of 200-230°C, and multi-stage precipitation involves many steps and various reagents. The separation yield and purity are not high , the process is long, the purity of recovered scandium and zirconium is not high, and the high-temperature process consumes a lot of energy

Method used

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  • Method for separating and recovering scandium in stable zirconia ceramic wastes containing scandium and rare earth

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Take 100 g of solid fuel cell (SOFC) ceramic waste, chemically composed of ZrO-containing 2 91%, Sc 2 o 3 7%, CeO 2 1.2%, Y 2 o 3 0.3% as raw material, first crush the above-mentioned waste to below 200 mesh, put it into a plastic king cup, add 500ml, 30%HF, soak at room temperature overnight, filter 610ml of filtrate, containing 141g / l ZrO2, the solution is heated and concentrated to When the volume is 280ml, add 100g solid KCl, stir evenly, cool, crystals are precipitated, and 190g KCl is obtained after draining 2 ZrF 6 , the recovery rate of zirconium is >90%, and the mother liquor is reserved for the next cycle.

[0032] ② After washing 87g of filter residue dissolved in HF, add 30ml of 8% NaOH solution, heat to temperature T=80°C, keep warm for 0.5 hours, cool and filter to obtain 12.45g of residue, wash the residue twice, add 10% 100ml of HCl, dissolve the slag, and obtain 2 o 3 62g / l, CeO 2 10g / l, Y 2 o 3 110ml of 2.6g / l solution, its acidity i...

Embodiment 2

[0037] Chemical composition is the ceramic powder waste material 100g with the embodiment 1, at first waste material is pulverized to below 200 orders, puts into plastic king cup, adds mixed acid (10%HF+5%H 2 SO 4 ) 600ml, heated to 80°C for 2 hours, cooled and filtered, the filtrate was heated, concentrated and crystallized as in Example 1, and the slag was washed with water, and the recovery and treatment steps of scandium and rare earth were the same as in Example 1.

Embodiment 3

[0039] Oxygen sensor zirconium-containing ceramic waste with a chemical composition of 92% ZrO 2 %, 8%Y 2 o 3 , first crush the waste to below -200 mesh, put it into a plastic bucket, add 20% HF, heat to temperature T=60°C, keep warm for 3hr, cool and filter, filtrate recovery, zirconium separation method is the same as in Example 1, filter After the residue is washed with water, use 10% NaOH solution at a temperature of 70°C, residue / liquid=1 / 2, conversion treatment time 1hr, cool and filter, wash the filter residue twice with water, dissolve HCl, control pH=1, add oxalic acid Precipitate yttrium. After the precipitate was washed, it was burned at 900°C for 3 hours to obtain yttrium oxide with a purity greater than 99%.

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Abstract

The invention discloses a method for separating and recovering scandium in stable zirconia ceramic wastes containing scandium and rare earth. The method comprises the following steps: crushing ceramic wastes firstly, sieving by virtue of a 200-mesh sieve, then dissolving the crushed powder by acid; after heating and concentrating a filtrate, adding potassium chloride, carrying out crystallization to obtain potassium fluozirconate, and separating zirconium from a solution; and washing filter residues, carrying out conversion treatment by using 5-20 percent sodium hydroxide, washing the residues again after treatment, dissolving with acid, extracting scandium by using an extractant so as to realize the separation of scandium and the rare earth, neutralizing an extraction raffinate with alkali, recovering the rare earth from precipitates, and searing to obtain rare earth oxide; and carrying out washing and back extraction on an organic phase for extracting the scandium, precipitating the scandium by oxalic acid, and searing to obtain scandium oxide. According to the method disclosed by the invention, the purity of Sc2O3 is larger than 99 percent, the recovery rate is larger than 90 percent, the recovery rate of the rare earth is larger than 90 percent, and the recovery rate of Zr is larger than 95 percent.

Description

technical field [0001] The invention relates to a method for separating and recovering scandium from zirconia ceramic waste containing scandium and rare earth stabilized. Background technique [0002] Rare earth-containing, especially scandium-containing stable zirconia ceramics have functions such as high hardness, electrical conductivity, and oxygen transport. They are widely used in solid fuel cells, oxygen sensors, artificial gemstones, etc., and recover valuable elements scandium, Rare earth and zirconium can realize the recovery of secondary resources, achieve the purpose of energy saving, emission reduction and recycling, which is in line with the national industrial policy of sustainable development. my country imports a large amount of zircon sand every year, reaching 800,000 tons per year, and has become the world's largest manufacturer of zirconium compounds. Waste of artificial gemstones (including ZrO 2 and Y 2 o 3 ) There are 400-600 tons of waste per year,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B7/00C22B59/00C22B34/14
CPCY02P10/20
Inventor 陈卫平彭业云王晓平
Owner HUNAN ORIENTAL SCANDIUM
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