WO2012163200A1 - Procédé de séparation de terres rares à partir d'un minerai de phosphore - Google Patents

Procédé de séparation de terres rares à partir d'un minerai de phosphore Download PDF

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Publication number
WO2012163200A1
WO2012163200A1 PCT/CN2012/074544 CN2012074544W WO2012163200A1 WO 2012163200 A1 WO2012163200 A1 WO 2012163200A1 CN 2012074544 W CN2012074544 W CN 2012074544W WO 2012163200 A1 WO2012163200 A1 WO 2012163200A1
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WIPO (PCT)
Prior art keywords
rare earth
acid
phosphoric acid
leaching
slag
Prior art date
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Ceased
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PCT/CN2012/074544
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English (en)
Chinese (zh)
Inventor
蒋开喜
冯林永
蒋训雄
汪胜东
范艳青
蒋伟
刘巍
张登高
王海北
张邦胜
林江顺
刘三平
赵磊
王玉芳
张磊
邹小平
黄胜
冯爱玲
蒋应平
冯亚平
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Beijing General Research Institute of Mining and Metallurgy
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Beijing General Research Institute of Mining and Metallurgy
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Publication of WO2012163200A1 publication Critical patent/WO2012163200A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

Definitions

  • This invention relates to the field of separating rare earths from rare earth-containing phosphate rock, and more particularly to a process for separating rare earths from phosphate rock. Background of the invention
  • the proven reserves of rare earth resources in the world are 45 million tons (in terms of oxides), which are relatively concentrated in China, the United States, India, Australia, the former Soviet Union and other countries.
  • Non-metallic phosphate ore is associated with a large amount of rare earth resources.
  • the total reserves of world phosphate rock is about 100 billion tons. According to the average content of rare earths, the total reserves are up to 50 million tons. It is important to recover rare earth from phosphate rock. .
  • the low content of rare earth in phosphate rock is not only economical for extracting rare earth raw materials, but also needs to be combined with the traditional phosphoric acid production process, that is, the recovery of rare earth in the process of producing phosphoric acid.
  • the production of wet-process phosphoric acid can be divided into: (1) hydrochloric acid method, (2) nitric acid method, and (3) sulfuric acid method.
  • the hydrochloric acid method is a method for early production of phosphoric acid.
  • the rare earth leaching rate is high, but the hydrochloric acid has strong volatility and severe corrosion to equipment, and the CaCl 2 solution treatment cost is relatively low in the process.
  • the wet method phosphoric acid is rarely used in the hydrochloric acid method. .
  • the nitric acid method has high leaching of rare earth and phosphorus in phosphate rock. From phosphate rock to pure rare earth phosphate, the recovery rate of rare earth can reach more than 85%. From phosphate rock to rare earth enrichment, the total yield can reach about 70%. . In addition, the method has little effect on the phosphorus chemical process and consumes less chemical raw materials, so the operation effect is good. However, the presence of nitric acid is expensive, and the extraction of rare earth by the nitric acid method does not have an economic advantage.
  • the sulfuric acid process is currently the main method for the production of wet process phosphoric acid in the world.
  • the rare earth can be controlled in phosphoric acid or controlled in phosphogypsum, so there are two processes of recovering rare earth from phosphoric acid and recovering rare earth from phosphogypsum.
  • Patent RU2225892C1 discloses the use of 20% to 25% sulfuric acid to leach rare earth from phosphogypsum.
  • Patent 200810068762 discloses a method for recovering rare earth from phosphogypsum, which uses 15% ⁇ 30% sulfuric acid to leach phosphogypsum to make rare earth into solution, and adds rare earth sulfate to solution to crystallize to obtain rare earth enrichment, and then use calcium nitrate.
  • Patent 200710053196 discloses a method for first leaching rare earth in phosphogypsum with sulfuric acid and ammonium sulfate solution, and then adding ammonia to adjust pH to recover rare earth.
  • US 4,636,369 discloses the introduction of aluminum ions, iron ions, silicon ions or mixed ions thereof in wet-process phosphoric acid slurries to increase the solubility of rare earths in solution, the highest enrichment of rare earths. The degree is 56%.
  • Patent 200710178377. 6 discloses the addition of an organic or inorganic surfactant to change the phosphogypsum crystal form during the decomposition of phosphate rock by sulfuric acid. The enrichment of rare earth in phosphoric acid can reach 80%.
  • Patent 200710179749 discloses a method for extracting rare earth from phosphoric acid and phosphogypsum by a precipitation method, respectively.
  • the rare earth phosphate rock and the return acid are slurried in the first chamber of the reaction tank, because the acid reflux temperature is 50. Above C, more than 50% of the rare earth in the phosphate rock enters the solution.
  • the sulfuric acid is added to the second, third and fourth tanks of the reaction tank, the rare earth will enter the phosphogypsum due to the adsorption of the phosphogypsum, because the amount of the phosphogypsum slag is large.
  • the rare earth grade is lower than the original ore. The process of recovering rare earth from phosphogypsum is complicated and economically difficult. Summary of the invention
  • the object of the present invention is to provide a method for separating rare earth from phosphate rock with a simple process, a low slag rate and a low cost in view of the deficiencies of the prior art.
  • Embodiments of the present invention provide a method of separating rare earth from phosphate rock, the method comprising the steps of:
  • a rare earth-containing phosphate concentrate is mixed with a phosphoric acid solution for reaction;
  • the phosphoric acid solution of the step (1) has a concentration of P 2 0 5 of 10% to 55%, preferably 15% to 20%; and the solid-liquid mass to volume ratio of the rare earth-containing phosphate concentrate and the phosphoric acid solution is 1
  • the reaction temperature is from 0.5 to 4 hours, and the reaction time is from 0.5 to 4 hours, preferably from 1 to 3 hours.
  • the acid leaching acid in the step (3) is one of sulfuric acid, hydrochloric acid, nitric acid and phosphoric acid, preferably sulfuric acid;
  • the sulfuric acid immersion temperature is 70-100 ° C, preferably 80-95 ° C ;
  • leaching The time is 0. 5- 5 hours, preferably 1-3 hours;
  • the leaching solid-liquid mass to volume ratio is 1: 2.
  • the acid amount is 1-4 times the theoretical acid consumption of calcium. 5 ⁇ Preferably, 1. 5-2. 5 times.
  • the method for separating rare earth from phosphate rock maintains the trend of the dominant element fluorine in the process of phosphoric acid leaching of phosphate rock, dissolves phosphorus in the phosphate rock and leaves the rare earth in the form of fluoride precipitate in the slag, thereby realizing the phosphate rock Efficient separation and enrichment of rare earths.
  • the method has the advantages of simple process, low slag rate, matching with wet phosphoric acid process, high precipitation rate of rare earth in phosphate rock and high rare earth grade in slag, and can realize low cost recovery of rare earth from rare earth phosphate rock.
  • the method for separating rare earth from phosphate rock comprises mixing rare earth-containing phosphorus concentrate with a certain concentration of phosphoric acid. With stirring, the phosphorus in the concentrate is leached into the solution, and the rare earth is left in the form of insoluble fluoride, and the filtrate and the rare earth-containing slag are separated by solid-liquid separation, and the filtrate enters the wet-process phosphoric acid production system to produce phosphoric acid or directly removes After the calcium is returned to the leaching, the rare earth in the slag is converted into a soluble rare earth salt by an acid, and then extracted by one or both of leaching, extraction, ion exchange adsorption, precipitation, and crystallization.
  • the method for separating rare earth from phosphate rock provided by the invention adopts phosphoric acid as a precipitating agent for rare earth in phosphate rock, and the phosphoric acid solution may be configured by industrial phosphoric acid, or may be a circulating dilute acid or a light phosphoric acid in the production process of wet process phosphoric acid. Phosphogypsum wash water, or a mixture of several of them.
  • the method for separating rare earth from phosphate rock comprises precipitating rare earth by adjusting process parameters, wherein the main phase of the slag is silica and a small amount of calcium fluoride, wherein the rare earth is mainly in the form of fluoride.
  • the extraction of rare earth from the slag can be carried out by a combination of various methods such as leaching, extraction, ion exchange adsorption, precipitation, and crystallization.
  • a rare earth element which may be a rare earth-containing phosphate rock and a rare earth-containing phosphate concentrate, in which the rare earth is richer than the rare earth in the ore. Therefore, it is economically more advantageous to treat rare earth-containing phosphate concentrates.
  • the method for separating rare earth from phosphate rock provided by the invention has the advantages of simple process, less slag rate, matching with wet process phosphoric acid process, high rare earth precipitation rate and high rare earth grade in slag.
  • the rare earth or phosphoric acid in the wet process phosphoric acid process can be used to precipitate the rare earth in the slag, which can be closely linked with the sulfuric acid process.
  • FIG. 1 is a process flow diagram of a method provided by an embodiment of the present invention. Mode for carrying out the invention
  • a method for separating rare earth from phosphate rock mixing a rare earth-containing phosphate concentrate with a phosphoric acid solution having a concentration of 10 ⁇ % - 55 ⁇ % ⁇ 2 0 5 according to a solid-liquid ratio of 1:4-10, and mixing the mixture at 15 O. 2-4 times the theoretical acid consumption of the calcium-containing slag is added to the slag of the rare earth-containing slag and the calcium-containing calcium.
  • Acid in the 70-100 ⁇ leaching 0. 5-5 hours, the slag in the rare earth into the solution, extraction method, ion exchange method, adsorption method, precipitation method, crystallization method, etc.
  • the phosphoric acid solution used is preferably a circulating dilute phosphoric acid, a light phosphoric acid or a phosphogypsum washing water in the phosphoric acid production process, and an insufficient portion can be supplemented with crude phosphoric acid.
  • rare earth-containing phosphorus concentrate containing 0.14% by mass of rare earth and ⁇ containing 20% of P 2 0 5 is diluted with 1:10, and the mixture is stirred at 15 ° C for 1 hour, and filtered.
  • the filtrate and the leaching slag are weighed and analyzed after drying.
  • the slag rate is 22%
  • the rare earth content in the slag is 0.59%
  • the rare earth is 93% enriched in the slag.
  • the enrichment ratio is 4.2 times.
  • the rare earth solution is subjected to recovery of rare earth by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • the mixed phosphoric acid solution containing P 2 0 5 is 2 (%) mixed at a solid-liquid ratio of 1:10, and stirred at 45 ° C for 1 hour, filtered. The filtrate and the leaching slag are obtained.
  • the leaching slag is dried and weighed and analyzed.
  • the slag rate is 21%, the rare earth content in the slag is 0.57%, and the rare earth is 85% enriched in the slag.
  • the enrichment ratio is 4.1 times, and the rare earth in the slag is leached with sulfuric acid.
  • the rare earth sulfate solution is subjected to recovery of rare earth by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • 100g of rare earth-containing phosphate concentrate containing 0.14 i of rare earth and 1000/ZZ diluted phosphoric acid solution containing P 2 0 5 of 20 i are mixed at a solid-liquid ratio of 1:10, stirred at 16 ° C for 4 hours, and filtered to obtain a filtrate.
  • leaching slag the leaching slag is dried, weighed and analyzed, the slag rate is 18%, the rare earth content in the slag is 0.73%, the rare earth 94% is enriched in the slag, the enrichment multiple is 5.2 times, and the rare earth slag is leached with sulfuric acid to obtain rare earth sulfate.
  • the solution is subjected to recovery of rare earth by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • the rare earth-containing phosphorus concentrate containing 0.14% ⁇ % of rare earth and 1000/ ⁇ dilute phosphoric acid solution containing P 2 0 5 of 20» ⁇ %, mix at a solid-liquid ratio of 1:5, and stir the reaction at 16 ° C for 4 hours.
  • the filtrate and the leaching slag are filtered, the leaching slag is dried, weighed and analyzed, the slag rate is 50%, the rare earth content in the slag is 0.27%, the rare earth is 95% enriched in the slag, and the enrichment ratio is 1.9 times.
  • the rare earth sulfate solution is leached, and the rare earth is recovered by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • 100g of rare earth-containing phosphate concentrate containing 0.14% of rare earth and 1000% of dilute phosphoric acid solution containing lanthanum are mixed at a solid-liquid ratio of 1:10, stirred at 16 ° C for 4 hours, filtered to obtain filtrate and leached.
  • the slag, the leaching slag is weighed and analyzed after drying, the slag rate is 41%, the rare earth content in the slag is 0.32%, the rare earth is 95% enriched in the slag, and the enrichment ratio is 2.3 times.
  • the rare earth slag is leached with sulfuric acid to obtain a rare earth sulfate solution.
  • the rare earth is recovered by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • 100 g of rare earth-containing phosphorus concentrate containing rare earth of 0.14 ⁇ % and 1000 mL of dilute phosphoric acid solution containing 20 ⁇ % are mixed at a solid-liquid ratio of 1:10, and stirred at 16 ° C for 4 hours, and filtered. ⁇
  • the enrichment factor is 6.8 times
  • the enrichment factor is 6.8 times
  • the enrichment factor is 6.8 times
  • the rare earth in the slag is leached with sulfuric acid to obtain a rare earth sulfate solution
  • the rare earth is recovered by one or more of an extraction method, an ion exchange adsorption method, a precipitation method, and a crystallization method.
  • the mixture of 100 g of rare earth slag and 700 sulphuric acid solution is mixed at a solid-liquid ratio of 1:7, and the amount of sulfuric acid is 2.5 times the theoretical acid consumption of calcium in the slag.
  • the reaction is stirred at 90 ° C for 2 hours, solid-liquid separation, gypsum residue drying. After weighing, analysis, the rare earth leaching rate is 90%, and the rare earth in the solution is recovered by one or more methods of extraction, ion exchange adsorption, precipitation, and crystallization.
  • the phosphoric acid solution of P 2 0 5 content 25 ⁇ % taken from a wet-process phosphoric acid plant is mixed with P 2 0 5 content 15%% phosphogypsum water to form a mixture of 1000 ⁇ P 2 0 5 quantity 20f ⁇ %.
  • Liquid take 100g of rare earth-containing phosphorus concentrate containing rare earth 0. 14 « ⁇ %, stir the reaction at 16 ° C for 4 hours, filter to obtain the filtrate, the filtrate is added with decalcification of sulfuric acid, which is 95% of the theoretical calcium acid consumption.
  • the decalcification solution is returned to the circulating leaching phosphorus under the same conditions, and the solid-liquid separation is performed.
  • the leaching slag is dried and weighed and analyzed, the slag rate is 30%, the rare earth content in the slag is 0.43%, and the rare earth 93% is enriched in the slag, rich
  • the set number is 3.1 times, and the rare earth in the slag is leached with sulfuric acid to obtain a rare earth sulfate solution, and the rare earth is recovered by one or more methods of extraction, ion exchange adsorption, precipitation, and crystallization.

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  • Chemical & Material Sciences (AREA)
  • Geology (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Life Sciences & Earth Sciences (AREA)
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  • Environmental & Geological Engineering (AREA)
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  • Metallurgy (AREA)
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  • Manufacture And Refinement Of Metals (AREA)
  • Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
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Abstract

La présente invention concerne un procédé de séparation de terres rares à partir d'un minerai de phosphore. Le procédé comprend les étapes consistant à : (1) mélanger et faire réagir le concentré de minerai de phosphore contenant des terres rares et une solution d'acide phosphorique ; (2) filtrer le mélange de façon à obtenir la solution de réaction et les scories contenant des terres rares ; (3) lixivier les scories contenant des terres rares en ajoutant de l'acide de façon à obtenir un lixiviat contenant des terres rares, puis recycler les terres rares selon un ou plusieurs procédés d'un processus d'extraction, un procédé d'adsorption et d'échange d'ions, un processus de précipitation et un processus de cristallisation, et (4) décalcifier la solution de réaction obtenue après le filtrage, puis revenir à l'étape (1). Dans le procédé de la présente invention, les terres rares extraites du minerai de phosphore présentent un taux de précipitation inférieur à 85 %, une faible efficacité des scories, une grande qualité des terres rares dans les scories et un fort taux de lixiviation des terres rares dans les scories. Le processus n'utilise pas d'additif. La qualité des produits à base d'acide phosphorique ne s'en ressent donc pas. L'acide phosphorique utilisé dans le processus peut être un acide phosphorique obtenu par auto-production. Il peut également s'agir d'un acide phosphorique dilué de recirculation, d'un acide faiblement phosphorique, etc., généré pendant une production d'acide phosphorique. Le procédé de la présente invention est étroitement lié au processus de production d'acide phosphorique utilisant de l'acide sulfurique.
PCT/CN2012/074544 2011-05-31 2012-04-23 Procédé de séparation de terres rares à partir d'un minerai de phosphore Ceased WO2012163200A1 (fr)

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CN201110143415A CN102220488B (zh) 2011-05-31 2011-05-31 一种从磷矿中分离稀土的方法

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CN102312089B (zh) * 2010-07-01 2013-06-05 北京矿冶研究总院 一种从含稀土的磷矿中回收稀土的方法
CN102220488B (zh) * 2011-05-31 2012-10-17 北京矿冶研究总院 一种从磷矿中分离稀土的方法
CN102796888B (zh) * 2012-09-09 2013-08-21 贵州黔鸿瑞磷稀土分裂开发有限公司 一种从磷精矿中提取稀土的工艺
CN103014359B (zh) * 2012-11-27 2014-03-19 益阳鸿源稀土有限责任公司 独居石渣的分离回收方法
CN105331812B (zh) * 2014-07-31 2018-03-16 有研稀土新材料股份有限公司 从含独居石稀土磷矿中综合回收磷和稀土的方法
CN105441674B (zh) * 2014-07-31 2017-10-13 有研稀土新材料股份有限公司 从含独居石磷矿中综合回收磷和稀土的方法
CN104150521B (zh) * 2014-08-06 2016-05-11 广东省工业技术研究院(广州有色金属研究院) 一种含稀土磷灰石矿回收磷和钙的方法
CN105525092B (zh) * 2014-09-30 2017-10-27 北京矿冶研究总院 一种含稀土磷矿通过优先浸出脱除磷钙富集稀土的方法
CN104532020B (zh) * 2014-12-11 2016-09-28 中国科学院长春应用化学研究所 从生产磷酸后的磷矿渣中回收稀土的方法
US10006102B2 (en) * 2015-01-08 2018-06-26 Institute Of Multipurpose Utilization Of Mineral Resources Monazite and apatite paragenetic ore enrichment method
AU2016200606B2 (en) * 2015-02-13 2021-05-13 Grirem Advanced Materials Co., Ltd A method for recovering phosphorus and rare earth from rare earth containing phosphorite
CN106319247B (zh) * 2015-06-19 2019-01-25 有研稀土新材料股份有限公司 从含稀土磷矿中回收磷和稀土的方法
AU2016279392B2 (en) * 2015-06-19 2019-01-31 Grirem Advanced Materials Co., Ltd. Method for recovering phosphorus and rare earth from rare earth-containing phosphate ore, and substance containing rare earth phosphate
CN105154689B (zh) * 2015-08-11 2017-09-12 贵州大学 一种磷矿中稀土分离富集的方法
CN105523533B (zh) * 2016-01-22 2017-12-15 贵州能矿织金磷化工有限公司 用再生磷酸浸取含稀土磷矿制取优质磷酸和优质磷石膏的方法
CN105543475B (zh) * 2016-02-03 2017-10-27 北京矿冶研究总院 从含稀土磷矿中富集和回收稀土的方法
CN107746977B (zh) * 2017-12-13 2019-11-01 济南大学 从含稀土磷矿中回收稀土的方法
CN112088224B (zh) 2018-05-03 2023-05-30 阿拉弗拉资源有限公司 稀土的回收方法
US11767228B2 (en) 2018-05-03 2023-09-26 Arafura Resources Limited Processing rare earth sulphate solutions
CN112080654B (zh) * 2020-09-25 2022-08-16 贵州省地质矿产中心实验室(贵州省矿产品黄金宝石制品质量检验站) 一种磷稀土化学精矿浸出液中回收酸和硅的方法
CN111979411A (zh) * 2020-09-25 2020-11-24 贵州省地质矿产中心实验室(贵州省矿产品黄金宝石制品质量检验站) 一种从含稀土磷矿中分离磷富集稀土的方法

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