CN103131862A - Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material - Google Patents
Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material Download PDFInfo
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Abstract
The invention relates to a pretreatment decomposition method for extracting high-purity rare earth oxide from a phosphor powder waste material. According to the pretreatment decomposition method, the phosphor powder waste material is subjected to the process flows of pretreatment, oxidizing roasting, acid hydrolysis, extraction, deposition and burning, and then the high-purity rare earth oxide is extracted. The reaction temperature is controlled, and a latent solvent is added, so that the recovery rate of rare earth in the waste material is improved; liquid caustic is used as a saponification extracting agent to achieve that waste water is discharged without ammonia and nitrogen, and the environmental pollution is reduced; and by adopting the method, the quality of a recovered product is improved, the production cost is reduced, and a process technology has a certain innovativeness.
Description
Technical field
The present invention relates to the recovery and utilization technology field of fluorescent powder scrap, be specially a kind of pre-treatment decomposition method and extract high purity rare earth oxides from fluorescent powder scrap.
Background technology
At present owing to producing and service factor, domesticly reach few hundred thousand tonnes of because of fluorescent material production and product rejection.The ubiquity ree distribution pattern differs in the middle of fluorescent powder scrap, have low taste and GOOD TASTE minute, yet, lowly sample that fluorescent powder scrap producer can only abandon or deposit it, can only process the GOOD TASTE fluorescent powder scrap.Reclaiming at present the production technique of valuable element normally from fluorescent powder scrap: the molten or alkali of roasting → acid soaks → purification and impurity removal → extracting and separating, purification.The molten yield of ubiquity rare earth waste material acid is low, and recovering rare earth chemical industry auxiliary material used has caused the waste of a large amount of valuable resources, and environment has been caused severe contamination finally with problems such as ammonia, the dischargings of nitrogen waste water formation.
Summary of the invention
Technical problem solved by the invention is to provide a kind of pre-treatment decomposition method to extract high purity rare earth oxides from fluorescent powder scrap, to solve the problem in the above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
The pre-treatment decomposition method is extracted high purity rare earth oxides from fluorescent powder scrap, comprise following 6 steps:
(1) fluorescent powder scrap pre-treatment; With fluorescent powder scrap add add water in the enamel reactor and stir after after the furnishing slurries, heat to 40～80 ℃; Slowly add hydrochloric acid to dissolve operation 12～20h to the enamel reactor, discharging supernatant liquor after clarification; Add again tap water to carry out the secondary removal of impurities, after completing, washing adds the pure rare earth solution stirring, add oxalic acid that the rare earth that is partly dissolved out is precipitated after constant temperature 20～40min, carry out filter press until put into plate-and-frame filter press during without rare earth element in the middle of the detection clear liquid, filtrate is to wastewater treatment, and filter cake is to oxidizing roasting;
(2) oxidizing roasting; After adding sodium hydroxide solution to mix through pre-treatment filter cake out, carry out roasting oxidation by kiln, controlling maturing temperature is 700～900 ℃, is incubated to the waste material roasting complete;
(3) acidolysis; In the molten tank of acid, the waste material after roasting is added water and make slurries, then add the hydrochloric acid dissolving, and add the solubility promoter hydrotropy, solution filters through plate-and-frame filter press and obtains rare earth chloride liquid, removal of impurities;
(4) extraction; Utilize liquid caustic soda as the extraction saponification agent, after dropping into liquid caustic soda in the rare earth chloride liquid and removal of impurities namely get rare-earth chloride solution, and reach waste water without ammonia, nitrogen discharged;
(5) precipitation; The rare-earth chloride solution that obtains to step (4) slowly drops into pure rare earth feed liquid and oxalic acid, and temperature is controlled 60 ℃～70 ℃, utilizes reactor and suction filtration pond to carry out rapid precipitation by precipitation agent and obtains rare earth oxalic acid thing;
(6) calcination; Utilize kiln to carry out 1000 ℃ of high temperature sinterings to the rare earth oxalic acid thing that step (5) obtains, then obtain high purity rare earth oxides through dehydration, carbonization, oxidation.
Beneficial effect:
The present invention has improved the rate of recovery of waste material middle-weight rare earths by controlling temperature of reaction and adding solubility promoter; Adopt liquid caustic soda as Saponified Extractants, reach waste water without ammonia, nitrogen discharged, alleviated environmental pollution; Improve and reclaim quality product, reduced production cost, Technology has certain novelty.
Embodiment
In order to make technique means of the present invention, creation characteristic, workflow, using method reach purpose and effect is easy to understand, below further set forth the present invention.
The pre-treatment decomposition method is extracted high purity rare earth oxides from fluorescent powder scrap, comprise following 6 steps:
(1) fluorescent powder scrap pre-treatment; Get the 300g fluorescent powder scrap and add in the enamel reactor, after adding 800ml water to stir the furnishing slurries, heat to 75 ℃; Slowly add hydrochloric acid to dissolve operation 20h to the enamel reactor, discharging supernatant liquor after clarification, add again tap water to carry out the secondary removal of impurities, after completing, washing adds the pure rare earth solution stirring, add oxalic acid that the rare earth that is partly dissolved out is precipitated after 75 ℃ of constant temperature 35min, carry out filter press until put into plate-and-frame filter press during without rare earth element in the middle of the detection clear liquid, filtrate is to wastewater treatment, and filter cake is to oxidizing roasting;
(2) oxidizing roasting; After adding sodium hydroxide solution to mix through pre-treatment filter cake out, carry out roasting oxidation by kiln, controlling maturing temperature is 700～900 ℃, is incubated to the waste material roasting complete;
(3) acidolysis; Add 1L water to make slurries in the waste material after roasting in the molten tank of acid, then add the hydrochloric acid dissolving, and add the solubility promoter hydrotropy, solution filters through plate-and-frame filter press and obtains rare earth chloride liquid, removal of impurities;
(4) extraction; Utilize liquid caustic soda as the extraction saponification agent, after dropping into liquid caustic soda in the rare earth chloride liquid, after mechanical stirring, removal of impurities namely gets rare-earth chloride solution, and reaches waste water without ammonia, nitrogen discharged;
(5) precipitation; The rare-earth chloride solution that obtains to step (4) slowly drops into pure rare earth feed liquid and oxalic acid, and temperature is controlled 65 ℃, utilizes reactor and suction filtration pond to carry out rapid precipitation by precipitation agent and obtains rare earth oxalic acid thing;
(6) calcination; Utilize kiln to carry out 1000 ℃ of high temperature sinterings to the rare earth oxalic acid thing that step (5) obtains, then obtain high purity rare earth oxides through dehydration, carbonization, oxidation.
Above demonstration and described ultimate principle of the present invention, principal character and advantage of the present invention.The technician of the industry should understand; the present invention is not restricted to the described embodiments; that describes in above-described embodiment and specification sheets just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (1)
1. pre-treatment decomposition method is extracted high purity rare earth oxides from fluorescent powder scrap, it is characterized in that: comprise following 6 steps:
(1) fluorescent powder scrap pre-treatment; With fluorescent powder scrap add add water in the enamel reactor and stir after after the furnishing slurries, heat to 40～80 ℃; Slowly add hydrochloric acid to dissolve operation 12～20h to the enamel reactor, discharging supernatant liquor after clarification; Add again tap water to carry out the secondary removal of impurities, after completing, washing adds the pure rare earth solution stirring, add oxalic acid that the rare earth that is partly dissolved out is precipitated after constant temperature 20～40min, carry out filter press until put into plate-and-frame filter press during without rare earth element in the middle of the detection clear liquid, filtrate is to wastewater treatment, and filter cake is to oxidizing roasting;
(2) oxidizing roasting; After adding sodium hydroxide solution to mix through pre-treatment filter cake out, carry out roasting oxidation by kiln, controlling maturing temperature is 700～900 ℃, is incubated to the waste material roasting complete;
(3) acidolysis; In the molten tank of acid, the waste material after roasting is added water and make slurries, then add the hydrochloric acid dissolving, and add the solubility promoter hydrotropy, solution filters through plate-and-frame filter press and obtains rare earth chloride liquid, removal of impurities;
(4) extraction; Utilize liquid caustic soda as the extraction saponification agent, after dropping into liquid caustic soda in the rare earth chloride liquid and removal of impurities namely get rare-earth chloride solution, and reach waste water without ammonia, nitrogen discharged;
(5) precipitation; The rare-earth chloride solution that obtains to step (4) slowly drops into pure rare earth feed liquid and oxalic acid, and temperature is controlled 60 ℃～70 ℃, utilizes reactor and suction filtration pond to carry out rapid precipitation by precipitation agent and obtains rare earth oxalic acid thing;
(6) calcination; Utilize kiln to carry out 1000 ℃ of high temperature sinterings to the rare earth oxalic acid thing that step (5) obtains, then obtain high purity rare earth oxides through dehydration, carbonization, oxidation.
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104946896A (en) * | 2015-07-15 | 2015-09-30 | 江西理工大学 | Method for extracting rare earth from waste rare earth phosphors |
| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN105200250A (en) * | 2015-09-30 | 2015-12-30 | 中铝广西国盛稀土开发有限公司 | Method of recovering rare-earth elements from oxalic acid precipitate rare-earth mother liquor |
| CN110627104A (en) * | 2019-08-30 | 2019-12-31 | 赣州市恒源科技股份有限公司 | Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
| CN111392756A (en) * | 2020-05-06 | 2020-07-10 | 龙南县中利再生资源开发有限公司 | Process for extracting high-purity rare earth oxide from fluorescent powder waste |
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| JPS61251514A (en) * | 1985-04-30 | 1986-11-08 | Mitsubishi Chem Ind Ltd | Method for recovering high-purity rare earth element oxide |
| JP2004285467A (en) * | 2003-01-27 | 2004-10-14 | National Institute Of Advanced Industrial & Technology | METHOD FOR SEPARATING AND RECOVERING Y AND Eu |
| CN102115822A (en) * | 2010-11-18 | 2011-07-06 | 吴泉锦 | Method for recovering rare earth oxide from fluorescent powder and polishing powder waste |
| CN102242270A (en) * | 2011-08-10 | 2011-11-16 | 于向真 | Method for recovering rare earth from catalyst waste residues |
| CN102634667A (en) * | 2012-04-26 | 2012-08-15 | 中国科学院城市环境研究所 | Method for recycling rear-earth elements form abandoned fluorescent lamps |
| CN102660688A (en) * | 2012-05-10 | 2012-09-12 | 北京科技大学 | Method for recovering rare earth from waste rare earth luminescent material |
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| JPS61251514A (en) * | 1985-04-30 | 1986-11-08 | Mitsubishi Chem Ind Ltd | Method for recovering high-purity rare earth element oxide |
| JP2004285467A (en) * | 2003-01-27 | 2004-10-14 | National Institute Of Advanced Industrial & Technology | METHOD FOR SEPARATING AND RECOVERING Y AND Eu |
| CN102115822A (en) * | 2010-11-18 | 2011-07-06 | 吴泉锦 | Method for recovering rare earth oxide from fluorescent powder and polishing powder waste |
| CN102242270A (en) * | 2011-08-10 | 2011-11-16 | 于向真 | Method for recovering rare earth from catalyst waste residues |
| CN102634667A (en) * | 2012-04-26 | 2012-08-15 | 中国科学院城市环境研究所 | Method for recycling rear-earth elements form abandoned fluorescent lamps |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105039698A (en) * | 2015-04-21 | 2015-11-11 | 南京林业大学 | Method of high-effectively recycling rare earth from waste CRT fluorescent powder |
| CN104946896A (en) * | 2015-07-15 | 2015-09-30 | 江西理工大学 | Method for extracting rare earth from waste rare earth phosphors |
| CN104946896B (en) * | 2015-07-15 | 2017-07-14 | 江西理工大学 | A kind of method of the Extraction of rare earth from useless fluorescent RE powder |
| CN105200250A (en) * | 2015-09-30 | 2015-12-30 | 中铝广西国盛稀土开发有限公司 | Method of recovering rare-earth elements from oxalic acid precipitate rare-earth mother liquor |
| CN110627104A (en) * | 2019-08-30 | 2019-12-31 | 赣州市恒源科技股份有限公司 | Method for preparing high-purity rare earth oxide by recovering fluorescent powder waste |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
| CN111392756A (en) * | 2020-05-06 | 2020-07-10 | 龙南县中利再生资源开发有限公司 | Process for extracting high-purity rare earth oxide from fluorescent powder waste |
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| CN103131862B (en) | 2016-09-14 |
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Address after: 341000 Fukang Industrial Zone, Longnan economic and Technological Development Zone, Longnan City, Ganzhou City, Jiangxi Province Patentee after: Longnan Zhongli renewable resources development Co.,Ltd. Address before: 341000 Fukang Industrial Zone, Longnan County, Ganzhou City, Jiangxi Province Patentee before: LONGNAN COUNTY ZHONGLI REGENERATION RESOURCE DEVELOPMENT Co.,Ltd. |