CN1405337A - Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid - Google Patents
Low-temperature roasting and decomposing process of rare earth heading concentrated sucfuric acid Download PDFInfo
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- CN1405337A CN1405337A CN02144405A CN02144405A CN1405337A CN 1405337 A CN1405337 A CN 1405337A CN 02144405 A CN02144405 A CN 02144405A CN 02144405 A CN02144405 A CN 02144405A CN 1405337 A CN1405337 A CN 1405337A
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- 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
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Abstract
The invention refers to a concentrated sulfuric acid low-temperature baking decomposing technique of rare-earth fine mineral. Mix the fine mineral and concentrated sulfurc acid in the weight proportion of 1:1.1-1:1.7, then bake it, and the baking temperature is 150-330 degree C (the optimum is 180-220 degree C); founder the baked mineral and filter it to get the leaching liquid and dregs; in the leaching liquid: the lixiviating rate of rare-earth is 95-98%, that of thorium >95%; in the leaching dregs: rare-earth <3%, thorium <3%; extract the leaching liquid to obtain thorium and rare-earth production.
Description
One, technical field:
The present invention relates to a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique.
Two, background technology:
At present, the main method of handling rare earth ore concentrate both at home and abroad is a vitriol oil high-temperature roasting method, and this method had obtained using widely in recent years.Though use this method can obtain certain economic benefits, " three wastes " problem that produces in vitriol oil high-temperature calcination process is difficult to solve.(1) waste residue: in vitriol oil high-temperature calcination process, the radioelement thorium mainly concentrates in the waste residue, belong to high slagging, this waste residue is difficult to dissolving and reclaims, many producers can only be stacked in the slag storehouse, cause the serious environmental pollution problem, the expense that is stored in the slag storehouse because of waste residue simultaneously is 0.25 yuan/kilogram, and this increases the burden of rare earth factory more.(2) waste gas: in vitriol oil high-temperature calcination process, produce a large amount of sulfur-bearings, fluorine, strongly-acid waste gas, contain obnoxious flavoures such as hydrogenchloride, sulfurous gas, sulphur trioxide in this waste gas, atmosphere is caused serious pollution.(3) waste water: in vitriol oil high-temperature calcination process, near the serious salinization in farmland making after the non-rare earth impurity discharging in the waste water, serious environment pollution.Except that above " three wastes " problem was difficult to solve, vitriol oil high-temperature roasting method also existed the problem that energy consumption is big, expense is high.Because above problems are not resolved, and cause some rare earth factories to shut down, stop, merge and change, and become the key issue that influences the Sustainable development of northern China rare earth.
Three, technology contents:
The objective of the invention is to exist waste residue, waste gas, waste water serious environment pollution at rare earth ore concentrate vitriol oil high-temperature roasting method, and insoluble problems such as energy consumption is big, provide a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, utilize this technology can reach (1) and make the thorium content in the waste residue drop to discharging standards, can build the dam discharging; (2) quantity discharged in the waste gas significantly reduces, and is convenient to recycling; (3) the detrimental impurity amount drops to minimumly in the waste water, does not cause environmental pollution.Adopt low-temperature bake technology, energy consumption cost also reduces greatly.For rare earth factory saves overspending.The present invention also aims to: rare earth ore concentrate is behind vitriol oil low-temperature bake, contain radioactive roasted ore after leaching dissolving, adopt extraction process that the radioelement thorium is focused on, both helped radioactive protection, can turn waste into wealth again, thorium be made the important source material product of nuclear industry.Other non-rare earth impurities also adopt corresponding technology to reclaim and produce corresponding product sale.
Rare earth ore concentrate vitriol oil low-temperature decomposition technology of the present invention, it is characterized in that rare earth ore concentrate and the vitriol oil by weight 1: 1.1-1: 1.7 mixed evenly forms sulfuric acid and mixes the ore deposit, and put into the retort furnace roasting, its maturing temperature is 150-330 ℃, its optimum calcination temperature is 180-220 ℃, forms roasted ore after roasting; Roasted ore is gone out, filters through water logging, obtain the infusion and the water logging slag of roasted ore, adopt extraction process to extract the thorium in the infusion, get rare-earth products after the separation.
Effect of the present invention is: rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, solved former high-temperature roasting technology indeterminable " three wastes " problem, and have following significant effect:
(1) the waste residue amount is reduced to half of former technology, its thorium content＜3%; Radioactivity always than put≤7.4 * 10
4Bq/Kg reaches the low slagging emission standard of country, can build the dam discharging, has saved waste residue is deposited in a large sum of expense in the slag storehouse.
(2) in the low-temperature bake process, decomposition reaction does not take place in sulfuric acid, and the tolerance of generation seldom is convenient to recycle with spraying process.
(3) in the low-temperature bake process, the roasted ore infusion, rare earth leaching yield 95-98%, thorium leaching yield＞95%, the thorium in the infusion can be used the extraction process extraction separation, produces the thorium product and recycles.Do not contain radioactivity (ThO in the rare-earth products that obtains simultaneously
2/ REO≤1 * 10
-5), there is not problem of environment pollution caused.
Four, embodiment:
Key problem in technology of the present invention is the preparation of roasted ore, and the weight ratio of promptly controlling the rare earth ore concentrate and the vitriol oil is 1: 1.1-1: within 1.7 the scope, and the control maturing temperature is between 150-330 ℃; All continue to use maturation process of the prior art from roasted ore to the extracting and separating that makes rare-earth products and thorium, so among the present invention this part technology is not described in detail.In fact, the roasted ore that makes by technology of the present invention goes out, filters through water logging, and the leaching yield of gained infusion middle-weight rare earths (in REO) is 95-98%, and thorium is (with ThO
2Meter) leaching yield is＞95%, and the water logging quantity of slag is half of the former high-temperature roasting quantity of slag that technology produces, water logging slag middle-weight rare earths＜3%, ThO
2＜3%, its radioactivity always than put≤7.4 * 10
4Bq/Kg has reached national low slagging emission standard.
Provide embodiments of the invention below:
Embodiment 1:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at 150 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore, filter then, obtain the infusion and the water logging slag of roasted ore.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 2:
(1) with a certain amount of rare earth ore concentrate (REO 〉=40%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at about 200 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 3:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, puts into the roasting ware, carries out roasting in retort furnace, and maturing temperature is controlled at 330 ℃.After 2 hours, take out the roasting ware, and roasted ore is weighed.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Embodiment 4:
(1) with a certain amount of rare earth ore concentrate (REO 〉=50%) and the vitriol oil with weight ratio 1: 1.1-1: 1.7 mixed is even, slowly adds to carry out roasting in the rotary kiln, and maturing temperature is controlled at 240-280 ℃.After after a while, effusive from the kiln tail both had been roasted ore.
(2) get a certain amount of roasted ore, add water, under certain temperature, carry out the aqueous solution leaching experiment of roasted ore,, obtain the infusion and the water logging slag of roasted ore through the water logging after-filtration of for some time.
(3) with infusion and water logging slag difference sampling analysis, in the infusion: the leaching yield of rare earth is 95-98%, and the leaching yield of thorium is＞95%; In the water logging slag: thorium＜3%, its radioactivity always are≤7.4 * 10 than putting
4Bq/Kg.
(4) infusion is carried out the extracting and separating thorium with extraction agent,, obtain thorium product and rare-earth products, do not contain radioactivity (ThO in the rare-earth products through extraction, washing, back extraction
2/ REO≤1 * 10
-5).
Claims (2)
1, a kind of rare earth ore concentrate vitriol oil low-temperature bake decomposition technique, it is characterized in that rare earth ore concentrate and the vitriol oil by weight 1: 1.1-1: 1.7 mixed evenly forms sulfuric acid and mixes the ore deposit, and put into the retort furnace roasting, its maturing temperature is 150-330 ℃, forms roasted ore after roasting; Roasted ore is gone out, filters through water logging, obtain the infusion and the water logging slag of roasted ore, adopt extraction process to extract the thorium in the infusion, get rare-earth products after the separation.
2, roasting decomposition technique according to claim 1 is characterized in that optimum calcination temperature is 180-220 ℃.
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| WO2009021389A1 (en) * | 2007-08-10 | 2009-02-19 | Grirem Advanced Materials Co., Ltd. | A PROCESS OF SMELTING MONAZITE RARE EARTH ORE RICH IN Fe |
| CN101824531A (en) * | 2010-03-12 | 2010-09-08 | 包头稀土研究院 | Liquid alkali low-temperature roasting decomposition process of caustic soda liquid of mixed rare earth concentrates |
| AU2008286599B2 (en) * | 2007-08-10 | 2010-11-18 | Grirem Advanced Materials Co., Ltd. | A metallurgical process for iron-rich monazite rare earth ore or concentrate |
| CN101899565A (en) * | 2009-05-31 | 2010-12-01 | 天津科技大学 | Process for decomposing Baotou rare earth ore concentrate and treating tail gas by medium-temperature reinforced roasting method |
| CN101492771B (en) * | 2009-03-04 | 2011-05-18 | 广州有色金属研究院 | Hingganite ore concentrate decomposition method |
| CN102094116A (en) * | 2011-02-21 | 2011-06-15 | 西安西骏新材料有限公司 | Device and method for decomposing rare earth ore through sulfuric acid low-temperature dynamic roasting |
| CN102864319A (en) * | 2011-10-08 | 2013-01-09 | 中国恩菲工程技术有限公司 | Method for leaching rare earth elements from nickel oxide ore |
| CN102876889A (en) * | 2012-09-29 | 2013-01-16 | 广州有色金属研究院 | Method for extracting rare earth from rare-earth-contained apatite ores |
| CN105568006A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Method for cleaning smelted mixed rare earth concentrate by concentrated sulfuric acid |
| CN106460087A (en) * | 2014-05-15 | 2017-02-22 | 淡水河谷公司 | System and process for selective rare earth extraction with sulfur recovery |
| CN106978532A (en) * | 2017-03-15 | 2017-07-25 | 包头稀土研究院 | The method that the concentrated sulfuric acid extracts fluorine-containing rare-earth mineral middle rare earth, fluorine and thorium |
| CN107267784A (en) * | 2017-07-17 | 2017-10-20 | 中国恩菲工程技术有限公司 | The system for handling rare earth ore concentrate |
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| CN108950188A (en) * | 2018-05-25 | 2018-12-07 | 包头稀土研究院 | The method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth |
| CN106978531B (en) * | 2017-03-15 | 2018-12-14 | 包头稀土研究院 | The method that soda acid joint decomposes mixed rare earth concentrate |
| CN109022838A (en) * | 2018-09-14 | 2018-12-18 | 包头稀土研究院 | The processing method of fluorine-containing rare-earth mineral particle |
| CN109988903A (en) * | 2019-05-21 | 2019-07-09 | 李梅 | A kind of method that concentrated sulfuric acid two-stage roasting decomposes high-grade mixed rare earth concentrates |
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- 2002-09-25 CN CNB021444056A patent/CN1173050C/en not_active Expired - Fee Related
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| WO2009021389A1 (en) * | 2007-08-10 | 2009-02-19 | Grirem Advanced Materials Co., Ltd. | A PROCESS OF SMELTING MONAZITE RARE EARTH ORE RICH IN Fe |
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| CN101899565A (en) * | 2009-05-31 | 2010-12-01 | 天津科技大学 | Process for decomposing Baotou rare earth ore concentrate and treating tail gas by medium-temperature reinforced roasting method |
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| CN109988903A (en) * | 2019-05-21 | 2019-07-09 | 李梅 | A kind of method that concentrated sulfuric acid two-stage roasting decomposes high-grade mixed rare earth concentrates |
| CN111187905A (en) * | 2020-02-11 | 2020-05-22 | 包头稀土研究院 | Method for decomposing mineral containing rare earth phosphate |
| CN111394571A (en) * | 2020-04-17 | 2020-07-10 | 包头稀土研究院 | Method for improving decomposition efficiency of rare earth mineral and sulfuric acid |
| CN111394571B (en) * | 2020-04-17 | 2022-02-15 | 包头稀土研究院 | Method for improving decomposition efficiency of rare earth mineral and sulfuric acid |
| CN113387381A (en) * | 2021-05-10 | 2021-09-14 | 江西铜业技术研究院有限公司 | Process for producing industrial precipitated barium sulfate by taking barite concentrate as raw material |
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| CN115058609A (en) * | 2022-06-20 | 2022-09-16 | 中国科学院地球化学研究所 | Method for leaching rare earth in basalt weathering crust |
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