CN104278164B - Grade is at the fluorine carbonated rare earth ore deposit of 62%-72% treatment process - Google Patents
Grade is at the fluorine carbonated rare earth ore deposit of 62%-72% treatment process Download PDFInfo
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- CN104278164B CN104278164B CN201410510876.0A CN201410510876A CN104278164B CN 104278164 B CN104278164 B CN 104278164B CN 201410510876 A CN201410510876 A CN 201410510876A CN 104278164 B CN104278164 B CN 104278164B
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Abstract
The invention discloses a kind of grade at the fluorine carbonated rare earth ore deposit of 62%-72% treatment process, comprise the steps: that (1) is by floating fluorine carbonated rare earth magnetic ore deposit dry 2-3 hour at 250-350 DEG C DEG C, (2) by floating dried magnetic ore deposit naked light calcination 6-8 hour at 400-600 DEG C, (3) 2-3 hour is reacted in floating the magnetic after calcination ore deposit under 1-1.5N hydrochloric acid system, obtain rare earth feed liquid and recrement, (4) recrement is transferred in high-temperature high-pressure reaction kettle, under 180-200g/L alkali lye system, react more than 4 hours, (5) by with alkali reaction after recrement be washed to neutrality, (6) recrement after washing is reacted to 2-3 hour under 2-2.5N hydrochloric acid system, obtain rare earth feed liquid and cerium enriched substance. the present invention has realized the best leaching in the floating ore deposit of magnetic. stop the condition that chlorine produces, made the safer environmental protection of production process. in the floating ore deposit of magnetic, major product praseodymium neodymium element leaching rate reaches more than 98%, far above original leaching level. making rare-earth smelting separate enterprise uses the overall economic efficiency in the floating ore deposit of magnetic greatly to improve.
Description
Technical field
The invention belongs to rare earth field, be specifically related to the treatment process in the floating ore deposit of a kind of Rare-Earth Magnetic.
Background technology
The floating ore deposit of Sichuan fluorine carbonated rare earth magnetic is without proprietary leaching technology now, and what each rare-earth smelting separated enterprise's employing is commonFluorine carbonated rare earth magnetic concentration hydrochloric acid system leaching technology.
Because existing fluorine carbonated rare earth head grade declines, particularly the floating ore deposit of grade magnetic between 62%-72%, passes through merelyThe rare earth ore concentrate of magnetic separation process enrichment can not meet gradually rare-earth smelting separate needs, and by magnetic separation flotation in conjunction with give birth toThe floating ore deposit of the magnetic of output is of high grade, and Costco Wholesale is low, but all the time in rare-earth smelting separating technology without specially for this kind of essenceThe smelting separating technology in ore deposit, causes the floating ore deposit of this kind of magnetic low at the production process middle rare earth yield that puts into operation, and operating cost is high, comprehensive warpJi benefit is on the contrary not as simple magnetic separation rare earth ore concentrate.
Summary of the invention
The object of the invention is to provide the floating ore deposit of a kind of magnetic treatment process, solves the floating mine disaster of the magnetic of grade between 62%-72% and soaksGet the not high problem of praseodymium neodymium yield.
Technical scheme of the present invention is: grade, at the fluorine carbonated rare earth ore deposit of 62%-72% treatment process, comprises the steps:
(1) grade is dried to 2-3 hour in the fluorine carbonated rare earth ore deposit of 62%-72% at 250-350 DEG C DEG C. Object is to removeContained moisture and decomposed fluorine carbonated rare earth in ore deposit, for the calcination in ore deposit provides good condition.
(2) by floating dried magnetic ore deposit naked light calcination 6-8 hour at 400-600 DEG C. By this temperature section calcination fluorineCarbonated rare earth ore deposit is converted into rare earth fluoride and rare earth oxide, according to the ore deposit transforming under experiment and this calcination condition of production checkingStone, easily, feed liquid cerium partition is low in leaching, and in cerium enriched substance, cerium partition is high.
(3) 2-3 hour is reacted in floating the magnetic after calcination ore deposit under 1-1.5N hydrochloric acid system, obtain rare earth feed liquid and recrement.Main leaching oxide part
(4) recrement is transferred in high-temperature high-pressure reaction kettle, under 180-200g/L alkali lye system, react 4 hours withOn. Mainly that rare earth fluoride is converted into rare earth hydrate.
(5) by with alkali reaction after recrement be washed to neutrality. Washing fluorine ion.
(6) recrement after washing is reacted to 2-3 hour under 2-2.5N hydrochloric acid system, obtain rare earth feed liquid and cerium enrichmentThing.
Further, its step is as follows:
(1) grade is dried to 3 hours in the fluorine carbonated rare earth ore deposit of 62%-72% at 250 DEG C,
(2) by the naked light calcination 6 hours at 420 DEG C of floating dried magnetic ore deposit,
(3) floating the magnetic after calcination ore deposit is reacted 2 hours under 1-1.5N hydrochloric acid system, obtains rare earth feed liquid and recrement,
(4) recrement is transferred in high-temperature high-pressure reaction kettle, under 180g/L alkali lye system, reacts 4 hours,
(5) by with alkali reaction after recrement be washed to neutrality,
(6) recrement after washing is reacted 2.5 hours under 2N hydrochloric acid system, obtain rare earth feed liquid and cerium enriched substance.
Further, its step is as follows:
(1) grade is dried to 2 hours in the fluorine carbonated rare earth ore deposit of 62%-72% at 300 DEG C,
(2) by the naked light calcination 7 hours at 460 DEG C of floating dried magnetic ore deposit,
(3) floating the magnetic after calcination ore deposit is reacted 3 hours under 1.5N hydrochloric acid system, obtains rare earth feed liquid and recrement,
(4) recrement is transferred in high-temperature high-pressure reaction kettle, under 200g/L alkali lye system, reacts 5 hours,
(5) by with alkali reaction after recrement be washed to neutrality,
(6) recrement after washing is reacted 2 hours under 2N hydrochloric acid system, obtain rare earth feed liquid and cerium enriched substance.
Further, its step is as follows:
(1) grade is dried to 2.5 hours in the fluorine carbonated rare earth ore deposit of 62%-72% at 350 DEG C,
(2) by the naked light calcination 8 hours at 500 DEG C of floating dried magnetic ore deposit,
(3) floating the magnetic after calcination ore deposit is reacted 2.5 hours under 1.5N hydrochloric acid system, obtains rare earth feed liquid and recrement,
(4) recrement is transferred in high-temperature high-pressure reaction kettle, under 190g/L alkali lye system, reacts 10 hours,
(5) by with alkali reaction after recrement be washed to neutrality,
(6) recrement after washing is reacted 3 hours under 2N hydrochloric acid system, obtain rare earth feed liquid and cerium enriched substance.
The present invention compared with prior art tool has the following advantages:
1, by the present invention, adjust calcination and the leaching condition in ore deposit, realize the best leaching in the floating ore deposit of magnetic. Original techniqueIn production process, easily produce chlorine, increased hydrochloric acid consumption. New technology has been stopped the condition that chlorine produces, and production process is more pacifiedLoopful is protected.
2, use technique of the present invention, in the floating ore deposit of magnetic, major product praseodymium neodymium element leaching rate reaches more than 98%, far above originalLeaching level.
3, use technique of the present invention, rare-earth smelting separates enterprise and uses the overall economic efficiency in the floating ore deposit of magnetic greatly to improve.
Detailed description of the invention
Embodiment 1
2000kg rawore REO66.7%, 250 DEG C are dried 3 hours, 420 DEG C of ripe ore deposit REO80% that calcination obtains for 6 hours.
Ripe ore deposit is added in retort and adds 1.5N hydrochloric acid reaction 2 hours, in slag, add 180g/L sodium hydroxide alkali to turn 4 littleTime, react rear extremely neutral with clear water washing, then added 2N hydrochloric acid reaction 2.5 hours, after having reacted, slag is used to clear water washingOnce, detect two excellent slags, REO78%La2O3/REO2.75%CeO2/REO95.2%Pr6O11/REO0.35%Nd2O3/REO0.95。
Embodiment 2
2000kg rawore REO67.76%, 300 DEG C are dried 2 hours, 460 DEG C of ripe ore deposit REO that calcination obtains for 7 hours78.45%。
Ripe ore deposit is added in retort and adds 1.5N hydrochloric acid reaction 3 hours, in slag, add 200g/L sodium hydroxide alkali to turn 5 littleTime, react rear extremely neutral with clear water washing, then added 2N hydrochloric acid reaction 2 hours, after having reacted, slag is used to clear water washing oneInferior, detect two excellent slags, REO86.88%La2O3/REO2.73%CeO2/REO95.85%Pr6O11/REO0.31%Nd2O3/REO0.89%。
Embodiment 3
2000kg rawore REO66.54%, 350 DEG C are dried 2.5 hours, 500 DEG C of ripe ore deposit REO that calcination obtains for 8 hours79.05%。
Ripe ore deposit is added in retort and adds 1.5N hydrochloric acid reaction 2.5 hours, in slag, add 190g/L sodium hydroxide alkali to turn10 hours, react rear extremely neutral with clear water washing, then added 2N hydrochloric acid reaction 3 hours, after having reacted, use clear water to wash slagWash once, detect two excellent slags, REO90.45%La2O3/REO2.70%CeO2/REO95.94%Pr6O11/REO0.21%Nd2O3/REO0.79%。
Embodiment 4
2000kg rawore REO70.54%, 350 DEG C are dried 2.4 hours, 480 DEG C of ripe ore deposit REO that calcination obtains for 7 hours83.05%。
Ripe ore deposit is added in retort and adds 1N hydrochloric acid reaction 2.3 hours, in slag, add 185g/L sodium hydroxide alkali to turn 9 littleTime, react rear extremely neutral with clear water washing, then added 2.5N hydrochloric acid reaction 3 hours, after having reacted, slag is used to clear water washingOnce, detect two excellent slags, REO92.45%La2O3/REO2.71%CeO2/REO95.84%Pr6O11/REO0.25%Nd2O3/REO0.82%。
The above embodiment has only expressed the application's detailed description of the invention, and it describes comparatively concrete and detailed, but alsoCan not therefore be interpreted as the restriction to the application's protection domain. It should be pointed out that for those of ordinary skill in the art, not departing under the prerequisite of present techniques plan plot, can also make some distortion and improvement, these all belong to thisThe protection domain of application.
Claims (1)
1. grade, at the fluorine carbonated rare earth ore deposit of 62%-72% treatment process, is characterized in that, its step is as follows:
(1) grade is dried to 2.5 hours in the fluorine carbonated rare earth ore deposit of 62%-72% at 350 DEG C,
(2) by the naked light calcination 8 hours at 500 DEG C of floating dried magnetic ore deposit,
(3) floating the magnetic after calcination ore deposit is reacted 2.5 hours under 1.5N hydrochloric acid system, obtains rare earth feed liquid and recrement,
(4) recrement is transferred in high-temperature high-pressure reaction kettle, under 190g/L alkali lye system, reacts 10 hours,
(5) by with alkali reaction after recrement be washed to neutrality,
(6) recrement after washing is reacted 3 hours under 2N hydrochloric acid system, obtain rare earth feed liquid and cerium enriched substance.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105331815B (en) * | 2015-10-15 | 2017-05-31 | 乐山盛和稀土股份有限公司 | The leaching technology of fluorine carbonated rare earth ore deposit |
| CN108034817B (en) * | 2017-10-31 | 2019-08-27 | 四川英创环保科技有限公司 | The technique that lime substitution liquid alkaline carries out alkali reaction in a kind of rare-earth smelting |
Citations (8)
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| CN1047110A (en) * | 1989-05-09 | 1990-11-21 | 兰州大学 | The novel method of from mishmetal, separating cerium dioxide |
| CN1103111A (en) * | 1993-11-26 | 1995-05-31 | 北京有色金属研究总院 | Making rare-earth material liquid from bastnae site |
| CN1103668A (en) * | 1993-12-07 | 1995-06-14 | 北京有色金属研究总院 | Method of extracting cerium-rich solution |
| CN1202460A (en) * | 1998-06-04 | 1998-12-23 | 葛新芳 | Method for producing mixed rare-earth chloride |
| CN101186967A (en) * | 2006-11-23 | 2008-05-28 | 贵州蓝天科大矿业发展有限公司 | Technique for comprehensive utilization clean production of phosphorus block ore and extracting rare earth form the phosphorus block ore |
| CN102399999A (en) * | 2010-09-15 | 2012-04-04 | 北京有色金属研究总院 | Comprehensive recovery process for rare earth and strontium intergrowth multi-metal ore |
| CN103225023A (en) * | 2013-04-26 | 2013-07-31 | 连云港市丽港稀土实业有限公司 | Method for leaching and recovering rare earth element from rare earth slag |
| CN103555943A (en) * | 2013-11-19 | 2014-02-05 | 乐山盛和稀土股份有限公司 | Mineral leaching process of bastnaesite |
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2014
- 2014-09-29 CN CN201410510876.0A patent/CN104278164B/en active Active
Patent Citations (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1047110A (en) * | 1989-05-09 | 1990-11-21 | 兰州大学 | The novel method of from mishmetal, separating cerium dioxide |
| CN1103111A (en) * | 1993-11-26 | 1995-05-31 | 北京有色金属研究总院 | Making rare-earth material liquid from bastnae site |
| CN1103668A (en) * | 1993-12-07 | 1995-06-14 | 北京有色金属研究总院 | Method of extracting cerium-rich solution |
| CN1202460A (en) * | 1998-06-04 | 1998-12-23 | 葛新芳 | Method for producing mixed rare-earth chloride |
| CN101186967A (en) * | 2006-11-23 | 2008-05-28 | 贵州蓝天科大矿业发展有限公司 | Technique for comprehensive utilization clean production of phosphorus block ore and extracting rare earth form the phosphorus block ore |
| CN102399999A (en) * | 2010-09-15 | 2012-04-04 | 北京有色金属研究总院 | Comprehensive recovery process for rare earth and strontium intergrowth multi-metal ore |
| CN103225023A (en) * | 2013-04-26 | 2013-07-31 | 连云港市丽港稀土实业有限公司 | Method for leaching and recovering rare earth element from rare earth slag |
| CN103555943A (en) * | 2013-11-19 | 2014-02-05 | 乐山盛和稀土股份有限公司 | Mineral leaching process of bastnaesite |
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Address after: 614803 Jinsu Town, Wutongqiao District, Leshan City, Sichuan Province Patentee after: Leshan Shenghe Rare Earth Co.,Ltd. Address before: 614803 Jinsu Town, Wutongqiao District, Leshan City, Sichuan Province Patentee before: LESHAN SHENGHE RARE EARTH Co.,Ltd. |