CN1173050C - Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate - Google Patents
Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate Download PDFInfo
- Publication number
- CN1173050C CN1173050C CNB021444056A CN02144405A CN1173050C CN 1173050 C CN1173050 C CN 1173050C CN B021444056 A CNB021444056 A CN B021444056A CN 02144405 A CN02144405 A CN 02144405A CN 1173050 C CN1173050 C CN 1173050C
- Authority
- CN
- China
- Prior art keywords
- rare earth
- thorium
- ore
- water
- temperature
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Expired - Fee Related
Links
Classifications
-
- 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
Landscapes
- Manufacture And Refinement Of Metals (AREA)
Abstract
本发明涉及一种稀土精矿浓硫酸低温焙烧分解工艺。将精矿与浓硫酸以重量比1∶1.1-1∶1.7的比例混合后进行焙烧，焙烧温度为150-330℃；将焙烧矿进行水浸、过滤，得到水浸液和水浸渣，水浸液中稀土的浸出率为95-98%，钍的浸出率为＞95%；水浸渣中：稀土＜3%，钍＜3%，其放射性总比放为≤7.4×104Bq/kg，且渣量少；将水浸液进行萃取提钍，得到钍产品和稀土产品，稀土产品中不含放射性(ThO2/REO≤1×10-5)。The invention relates to a rare earth concentrate concentrated sulfuric acid roasting decomposition process at low temperature. The concentrated ore and concentrated sulfuric acid are mixed in a weight ratio of 1:1.1-1:1.7 and then roasted at a temperature of 150-330°C; the roasted ore is soaked in water and filtered to obtain water immersion liquid and water leaching slag, water The leaching rate of rare earth in the leaching solution is 95-98%, and the leaching rate of thorium is >95%; in the water leaching residue: rare earth <3%, thorium <3%, and its total radioactivity ratio is ≤7.4×10 4 Bq/ kg, and the amount of slag is small; extract thorium from the water immersion solution to obtain thorium products and rare earth products, and the rare earth products do not contain radioactivity (ThO 2 /REO≤1×10 -5 ).
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 hydrogen fluoride, 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 maturing 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 maturing temperature is 180-220 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021444056A CN1173050C (en) | 2002-09-25 | 2002-09-25 | Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021444056A CN1173050C (en) | 2002-09-25 | 2002-09-25 | Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1405337A CN1405337A (en) | 2003-03-26 |
| CN1173050C true CN1173050C (en) | 2004-10-27 |
Family
ID=4750562
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB021444056A Expired - Fee Related CN1173050C (en) | 2002-09-25 | 2002-09-25 | Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN1173050C (en) |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
Families Citing this family (23)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2009021389A1 (en) * | 2007-08-10 | 2009-02-19 | Grirem Advanced Materials Co., Ltd. | A PROCESS OF SMELTING MONAZITE RARE EARTH ORE RICH IN Fe |
| CN101363079A (en) * | 2007-08-10 | 2009-02-11 | 有研稀土新材料股份有限公司 | Smelting method of iron rich mengite rare-earth mine |
| CN101492771B (en) * | 2009-03-04 | 2011-05-18 | 广州有色金属研究院 | Hingganite ore concentrate decomposition method |
| CN101899565A (en) * | 2009-05-31 | 2010-12-01 | 天津科技大学 | Decomposition of Baotou Rare Earth Concentrate and Tail Gas Treatment Process by Medium Temperature Intensified Roasting |
| 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 |
| CN102094116B (en) * | 2011-02-21 | 2012-07-04 | 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 |
| CN102864319B (en) * | 2011-10-08 | 2015-02-04 | 中国恩菲工程技术有限公司 | Method for leaching rare earth elements from nickel oxide ore |
| CN102876889B (en) * | 2012-09-29 | 2014-05-07 | 广州有色金属研究院 | Method for extracting rare earth from rare-earth-contained apatite ores |
| US10597754B2 (en) * | 2014-05-15 | 2020-03-24 | Vale S.A. | System and process for selective rare earth extraction with sulphur recovery |
| 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 |
| 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 |
| 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 |
| CN107267784B (en) * | 2017-07-17 | 2022-09-20 | 中国恩菲工程技术有限公司 | System for handle rare earth concentrate |
| CN107475542B (en) * | 2017-07-17 | 2021-03-16 | 中国恩菲工程技术有限公司 | Method for treating rare earth concentrate |
| CN108950188B (en) * | 2018-05-25 | 2020-06-30 | 包头稀土研究院 | Method for step-by-step extraction of phosphorus and rare earth from concentrated sulfuric acid low-temperature roasting phosphorus-containing rare earth concentrate |
| CN109022838B (en) * | 2018-09-14 | 2020-03-06 | 包头稀土研究院 | Method for treating fluorine-containing rare earth mineral particles |
| 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 |
| 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 |
| CN113528844B (en) * | 2021-07-15 | 2022-12-06 | 江西理工大学 | Method for efficiently separating valuable metals from copper regeneration soot |
| CN115058609A (en) * | 2022-06-20 | 2022-09-16 | 中国科学院地球化学研究所 | A method for leaching rare earth from basalt weathering crust |
| CN115159594B (en) * | 2022-08-01 | 2024-05-14 | 中伟新材料股份有限公司 | Method for preparing metal sulfate |
-
2002
- 2002-09-25 CN CNB021444056A patent/CN1173050C/en not_active Expired - Fee Related
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
Also Published As
| Publication number | Publication date |
|---|---|
| CN1405337A (en) | 2003-03-26 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN1173050C (en) | Low-temperature Roasting Decomposition Technology of Concentrated Sulfuric Acid for Rare Earth Concentrate | |
| CN111020193B (en) | Method for recovering vanadium, tungsten and titanium elements from waste SCR denitration catalyst | |
| CN100357464C (en) | Technology of preparing fluorine less niobium oxide by oxalic acid system extraction method | |
| CN103667728B (en) | The method of scandium is reclaimed from red mud slag | |
| WO2014082461A1 (en) | Monazite ballast separation and recovery method | |
| CN101092248A (en) | Technique for producing vanadium pentoxide | |
| CN103233125A (en) | Method for extracting tungsten, molybdenum and rhenium from waste high-temperature alloy | |
| CN104120268A (en) | Method for extracting scandium from waste titanium dioxide acid and bayer method red mud in normal pressure at low temperature | |
| Liu et al. | Thorough extraction of lithium and rubidium from lepidolite via thermal activation and acid leaching | |
| CN105039724B (en) | Smelting furnace soot treatment method | |
| CN101392332A (en) | A clean production process for the direct conversion and extraction of rare earths from sulfuric acid rare earth roasted ore | |
| CN104120267A (en) | Method for extracting high-purity scandium oxide from titanium dioxide waste acid and Bayer-process red mud by virtue of high-temperature acid leaching | |
| CN108950217A (en) | A method of recycling gold and silver from waste printed circuit board | |
| CN100554445C (en) | A kind of inclined to one side potassium tantalate, method of tantalum and niobium in the potassium niobate mixture partially of separating | |
| CN106337134A (en) | Technique for recovering indium from indium-containing soot | |
| CN1940096A (en) | Extraction of vanadium and molybdenum compound from refused materials containing vanadium and molybdenum etc. multiple elements | |
| CN103014316A (en) | Novel method for processing lepidolite material | |
| CN103014358B (en) | Treatment method of tailings after separation and recovery of monazite slag | |
| CN108950218A (en) | A method of recycling gold, silver and copper from waste printed circuit board | |
| Soisson et al. | Staff-industry collaborative report tantalum and niobium | |
| CN111593213A (en) | Method for extracting rare earth from rare earth organic slag | |
| CN102976382B (en) | A method for regenerating cryolite from electrolytic aluminum waste | |
| CN117208952A (en) | Preparation method of yttrium oxide | |
| CN111732123B (en) | Method for preparing magnesium metavanadate from waste SCR denitration catalyst | |
| CN103451452A (en) | Method for recovering tin from tin-containing waste liquid |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C14 | Grant of patent or utility model | ||
| GR01 | Patent grant | ||
| C17 | Cessation of patent right | ||
| CF01 | Termination of patent right due to non-payment of annual fee |
Granted publication date: 20041027 Termination date: 20130925 |