CN105543509A - Method for preparing rare earth chloride from mixed rare earth concentrate or bastnaesite concentrate - Google Patents
Method for preparing rare earth chloride from mixed rare earth concentrate or bastnaesite concentrate Download PDFInfo
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- CN105543509A CN105543509A CN201610000533.9A CN201610000533A CN105543509A CN 105543509 A CN105543509 A CN 105543509A CN 201610000533 A CN201610000533 A CN 201610000533A CN 105543509 A CN105543509 A CN 105543509A
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- rare earth
- concentrate
- hamartite
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- hydrochloric acid
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Classifications
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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
-
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- 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
Abstract
The invention relates to a method for preparing rare earth chloride from mixed rare earth concentrate or bastnaesite concentrate and belongs to the field of hydrometallurgy. The method is implemented according to the following steps that firstly, the mixed rare earth concentrate with the rare earth grade of 62%-70% or the bastnaesite concentrate is directly subjected to hydrochloric acid leaching; secondly, acid leaching residues obtained after hydrochloric acid leaching is subjected to alkali decomposion; thirdly, washing is conducted to remove impurity elements such as fluorine and phosphorus, and alkali, fluorine and phosphorus are recovered from washing liquid; fourthly, washing residues and acid leaching liquid obtained from the first step are mixed for acid leaching; and finally, the acid leaching liquid is neutralized, iron and thorium are removed, and a qualified mixed rare earth chloride solution is obtained. The method has the beneficial effects that the roasting link with high energy consumption is omitted, a large amount of acid gas of sulfur and fluorine and ammonia nitrogen waste water cannot be generated, and labor protection and environment protection are facilitated; and valuable elements are comprehensively recycled, the alkali consumption amount is small, cost is low, the rare earth recovery rate is high, and three-waste pollution is avoided.
Description
Technical field
The present invention relates to a kind of method that mixed rare earth concentrate or fluoro-carbon-cerium ore concentrate prepare rare earth chloride, belong to field of hydrometallurgy.
Background technology
Mainly hamartite (REFCO in the mixed rare earth concentrate of packet header
3) and monazite (REPO
4) mineral association of two kinds of mineral, with its association also have the mineral such as fluorite, calcite, phosphatic rock.This ore deposit mineral composition is complicated, and disseminated grain size is thin, is typical difficult point of smelting mineral of solving problem.
At present, study the third generation concentrated sulfuric acid roasting technique of total institute independent development in industrial production based on Beijing non-ferrous metal, sodium hydroxide decomposition method is auxiliary.The major advantage of concentrated sulfuric acid roasting method is that rare earth grade requirement is low, technique is simple, flow process is short, be convenient to scale operation, but along with country is to the attention of comprehensive utilization of resources and environmental issue, this technique Problems existing is also more and more outstanding: multiple valuable element can not get efficient recovery, three-waste pollution problem is difficult to basic solution, thorium exists with the form of pyrophosphate salt, is difficult to process and reclaims, must deposit specially.The requirement that the defect existed due to this technique self and country discharges three-waste pollution is more and more stricter, and concentrated sulfuric acid roasting technique faces the edge being about to be eliminated, need badly the new smelting technology developing a kind of clean and effective substitute.
Mixed rare earth concentrates another important smelting technology in packet header is sodium hydroxide decomposition method.This technique is needs blanking calcium first, then washing filtering, then decompose with liquid caustic soda, and then washing is except soluble salts such as lixiviating, sodium phosphate, Sodium Fluorides, and last Leaching in Hydrochloric Acid obtains re chloride.This technique, compared with acid technological process, is a kind of technique of clean, efficient, resource comprehensive utilization, but there is following subject matter: operational process of craft is discontinuous, and alkali consumption is large, and water resource waste is large, and production cost is high, and equipment corrosion is serious.
Summary of the invention
The object of this invention is to provide a kind of clean and effective and the mixed rare earth concentrates of synthetical recovery various valuable element or fluoro-carbon-cerium ore concentrate can prepare the method for rare earth chloride, the method eliminates the higher roasting link of energy consumption, synthetical recovery valuable element, rare earth yield is high, three-waste free pollution.
The present invention seeks to realize with under type:
The method major technique step that mixed rare earth concentrates or fluoro-carbon-cerium ore concentrate prepare rare earth chloride comprises: first mixed rare earth concentrates or hamartite are directly carried out Leaching in Hydrochloric Acid, then sodium hydroxide is adopted to carry out caustic digestion to acid leaching residue, temperature during caustic digestion controls at 150 ~ 250 DEG C, 1 ~ 2 hour time; Finally by washing, acidleach, neutralization, the neutralizer obtained is re chloride, and rare earth yield, more than 95%, is iron thorium slag with slag in obtaining.
The present invention adopts Leaching in Hydrochloric Acid: by REO be 62% ~ 70% mixed rare earth concentrates or hamartite directly carry out Leaching in Hydrochloric Acid, concentration of hydrochloric acid 6 ~ 12mol/L, solid-to-liquid ratio is 1:1.5 ~ 10, extraction temperature is 70 ~ 100 DEG C, 1 ~ 3 hour time, the pickling liquor I obtained and acid leaching residue I carry out sealing up for safekeeping for subsequent use.
Further: in caustic digestion process, the mass concentration of sodium hydroxide is 50% ~ 75%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:0.7 ~ 1.5.Finally by washing, acidleach, neutralization, the neutralizer obtained is re chloride, and rare earth yield, more than 95%, is iron thorium slag with slag in obtaining.
Described mixed rare earth concentrates or fluoro-carbon-cerium ore concentrate are the mixed rare earth concentrate of the hamartite of REO grade between 62% ~ 70% and solitary stone ore or independent hamartite.
Advantage of the present invention
1. this technique eliminates the firing stage in traditional acid technological process, reduces energy consumption, can not produce sour gas and the ammonia nitrogen waste water of a large amount of sulphur and fluorine, be conducive to labor protection and environment protection.
2. this technique achieves the comprehensive reutilization of resource, and can reclaim the raw material that sodium hydroxide is used as caustic digestion in water lotion, the Sodium Fluoride simultaneously reclaimed and sodium phosphate reach national standard, and thorium exists with the form of thorium enriched thing, can as the raw material carrying thorium.
This technique alkali consumption is few, and cost is low, and rare earth yield is high, and is applicable to the mixed rare earth concentrate of hamartite and solitary stone ore or independent hamartite.
The present invention adopts the method directly leached, and not only achieves the high-recovery that rare earth leaches, reaches the object that hamartite is separated with monazite simultaneously, carry out caustic digestion process further again to monazite.Whole rational technology arranges each operational phase, and eliminate the roasting link that energy consumption is higher, synthetical recovery valuable element, rare earth leaching yield is high, stops three-waste pollution.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Introduce technical scheme of the present invention in detail below by specific embodiment, but claim of the present invention is not limited to the following examples.
Embodiment 1
(1) Leaching in Hydrochloric Acid: get 5kgREO be 62.5% directly carry out Leaching in Hydrochloric Acid based on the mixed rare earth concentrate of hamartite and solitary stone ore, concentration of hydrochloric acid 6mol/L, solid-to-liquid ratio is 1:3, and extraction temperature is 80 DEG C, time 2 h, the pickling liquor I obtained and acid leaching residue I;
(2) caustic digestion: adopt sodium hydroxide to carry out caustic digestion to the acid leaching residue I that (1) step obtains, the concentration of sodium hydroxide is 70%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:1, and temperature during caustic digestion controls at 230 DEG C, 1 hour time;
(3) wash: wash caustic digestion mineral with general industry water, washing temperature is 80 DEG C, filters when being washed to pH=8;
(4) acidleach: joined by the washing slag that (3) step obtains in the pickling liquor I that (1) step obtains, mix and blend, temperature controls at 80 DEG C, and solid-to-liquid ratio is 1:5;
(5) neutralize: the ammonia soln slowly adding concentration 10% in the pickling liquor II that (4) step obtains, stir, temperature controls at 60 DEG C, adjustment pH to 4.0, churning time is 0.5 hour, and the neutralizer obtained is re chloride, REO content is 235.74g/L, rare-earth yield is 96.15%, is iron thorium slag in obtaining with slag, and sealing is preserved.
Embodiment 2
(1) Leaching in Hydrochloric Acid: get 5kgREO be 65.85% fluoro-carbon-cerium ore concentrate directly carry out Leaching in Hydrochloric Acid, concentration of hydrochloric acid 8mol/L, solid-to-liquid ratio is 1:2.5, and extraction temperature is 80 DEG C, 1.5 hours time, the pickling liquor I obtained and acid leaching residue I;
(2) caustic digestion: adopt sodium hydroxide to carry out caustic digestion to the acid leaching residue I that (1) step obtains, the concentration of sodium hydroxide is 65%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:1, and temperature during caustic digestion controls at 220 DEG C, 1 hour time;
(3) wash: wash caustic digestion mineral with general industry water, washing temperature is 60 DEG C, filters when being washed to pH=8.5;
(4) acidleach: joined by the washing slag that (3) step obtains in the pickling liquor I that (1) step obtains, mix and blend, temperature controls at 60 DEG C, and solid-to-liquid ratio is 1:5;
(5) neutralize: the ammonia soln slowly adding concentration 15% in the pickling liquor II that (4) step obtains, stir, temperature controls at 55 DEG C, adjustment pH to 3.8, churning time is 0.5 hour, and the neutralizer obtained is re chloride, REO content is 226.35g/L, rare-earth yield is 95.72%, is iron thorium slag in obtaining with slag, and sealing is preserved.
Embodiment 3
(1) Leaching in Hydrochloric Acid: get 5kgREO be 66.48% directly carry out Leaching in Hydrochloric Acid based on the mixed rare earth concentrate of hamartite and solitary stone ore, concentration of hydrochloric acid 10mol/L, solid-to-liquid ratio is 1:3, and extraction temperature is 50 DEG C, 1 hour time, the pickling liquor I obtained and acid leaching residue I;
(2) caustic digestion: adopt sodium hydroxide to carry out caustic digestion to the acid leaching residue I that (1) step obtains, the concentration of sodium hydroxide is 70%, consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:0.8, and temperature during caustic digestion controls at 200 DEG C, 1.5 hours time;
(3) wash: wash caustic digestion mineral with general industry water, washing temperature is 55 DEG C, filters when being washed to pH=8;
(4) acidleach: joined by the washing slag that (3) step obtains in the pickling liquor I that (1) step obtains, mix and blend, temperature controls at 75 DEG C, and solid-to-liquid ratio is 1:8;
(5) neutralize: the sodium hydroxide solution slowly adding concentration 5% in the pickling liquor II that (4) step obtains, stir, temperature controls at 80 DEG C, adjustment pH to 4.5, churning time is 1.5 hours, and the neutralizer obtained is re chloride, REO content is 247.26g/L, rare-earth yield is 97.33%, is iron thorium slag in obtaining with slag, and sealing is preserved.
Embodiment 4
(1) Leaching in Hydrochloric Acid: get 5kgREO be 68.29% directly carry out Leaching in Hydrochloric Acid based on the mixed rare earth concentrate of hamartite and solitary stone ore, concentration of hydrochloric acid 7mol/L, solid-to-liquid ratio is 1:8, and extraction temperature is 35 DEG C, time 2 h, the pickling liquor I obtained and acid leaching residue I;
(2) caustic digestion: adopt sodium hydroxide to carry out caustic digestion to the acid leaching residue I that (1) step obtains, the concentration of sodium hydroxide is 75%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:1.2, and temperature during caustic digestion controls at 250 DEG C, time 2 h;
(3) wash: wash caustic digestion mineral with general industry water, washing temperature is 90 DEG C, filters when being washed to pH=9;
(4) acidleach: joined by the washing slag that (3) step obtains in the pickling liquor I that (1) step obtains, mix and blend, temperature controls at 70 DEG C, and solid-to-liquid ratio is 1:10;
(5) neutralize: the sodium hydroxide solution slowly adding concentration 10% in the pickling liquor II that (4) step obtains, stir, temperature controls at 60 DEG C, adjustment pH to 4.2, churning time is 1 hour, and the neutralizer obtained is re chloride, REO content is 223.96g/L, rare-earth yield is 95.89%, is iron thorium slag in obtaining with slag, and sealing is preserved.
Embodiment 5
(1) Leaching in Hydrochloric Acid: get 5kgREO be 70.15% fluoro-carbon-cerium ore concentrate directly carry out Leaching in Hydrochloric Acid, concentration of hydrochloric acid 11mol/L, solid-to-liquid ratio is 1:4, and extraction temperature is 85 DEG C, 1.5 hours time, the pickling liquor I obtained and acid leaching residue I;
(2) caustic digestion: adopt sodium hydroxide to carry out caustic digestion to the acid leaching residue I that (1) step obtains, the concentration of sodium hydroxide is 55%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:0.8, and temperature during caustic digestion controls at 185 DEG C, time 2 h;
(3) wash: wash caustic digestion mineral with general industry water, washing temperature is 40 DEG C, filters when being washed to pH=9;
(4) acidleach: joined by the washing slag that (3) step obtains in the pickling liquor I that (1) step obtains, mix and blend, temperature controls at 80 DEG C, and solid-to-liquid ratio is 1:12;
(5) neutralize: the sodium hydroxide solution slowly adding concentration 25% in the pickling liquor II that (4) step obtains, stir, temperature controls at 80 DEG C, adjustment pH to 4.0, churning time is 1.5 hours, and the neutralizer obtained is re chloride, REO content is 235.48g/L, rare-earth yield is 96.77%, is iron thorium slag in obtaining with slag, and sealing is preserved.
Claims (4)
1. the method for rare earth chloride prepared by mixed rare earth concentrate or hamartite, it is characterized in that, its method is as follows: mixed rare earth concentrates or hamartite are directly carried out Leaching in Hydrochloric Acid, sodium hydroxide solution is adopted to carry out caustic digestion to acid leaching residue, temperature during caustic digestion controls at 150 ~ 250 DEG C, 1 ~ 2 hour time; Through washing, acidleach, neutralization, the neutralizer obtained is qualified re chloride, and rare earth yield, more than 95%, is iron thorium slag with slag in obtaining.
2. the method for rare earth chloride prepared by mixed rare earth concentrate according to claim 1 or hamartite, it is characterized in that, Leaching in Hydrochloric Acid: by REO be 62% ~ 70% mixed rare earth concentrates or hamartite directly carry out Leaching in Hydrochloric Acid, concentration of hydrochloric acid 6 ~ 12mol/L, solid-to-liquid ratio is 1:1.5 ~ 10, extraction temperature is 70 ~ 100 DEG C, 1 ~ 3 hour time, and the pickling liquor I obtained and acid leaching residue I carry out sealing up for safekeeping for subsequent use.
3. the method for rare earth chloride prepared by mixed rare earth concentrate according to claim 1 or hamartite, it is characterized in that, in caustic digestion process, the mass concentration of sodium hydroxide is 50% ~ 75%, and consumption is: rare earth ore concentrate quality: sodium hydroxide quality=1:0.7 ~ 1.5.
4. the method for rare earth chloride prepared by mixed rare earth concentrate according to claim 1 and 2 or hamartite, it is characterized in that, described mixed rare earth concentrate or fluoro-carbon-cerium ore concentrate are the mixed rare earth concentrate of the hamartite of REO grade between 62% ~ 70% and solitary stone ore or independent hamartite.
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Cited By (14)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803187A (en) * | 2016-05-19 | 2016-07-27 | 东北大学 | Microwave-assisted decomposition method for Baotou mixed rare earth concentrates |
| CN106801153A (en) * | 2016-12-30 | 2017-06-06 | 包头稀土研究院 | A kind of method of low cost enrichment high-grade mixed rare earth concentrates |
| CN106916975A (en) * | 2017-03-07 | 2017-07-04 | 四川省冕宁县方兴稀土有限公司 | A kind of method of Extraction of rare earth in thorium waste residue from iron |
| 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 |
| 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 |
| CN109266838A (en) * | 2017-07-18 | 2019-01-25 | 有研稀土新材料股份有限公司 | The processing method of bastnaesite and the composite ore containing bastnaesite |
| CN110512098A (en) * | 2019-08-29 | 2019-11-29 | 包头钢铁（集团）有限责任公司 | A kind of method that bastnaesite wet process prepares rare earth chloride |
| CN111187926A (en) * | 2020-01-07 | 2020-05-22 | 包钢集团矿山研究院（有限责任公司） | Method for hydrometallurgical smelting of baiyuneboite concentrate |
| CN111636001A (en) * | 2020-05-19 | 2020-09-08 | 四川省冕宁县方兴稀土有限公司 | Acid-base combined method for treating bastnaesite and recovering rare earth from waste slag |
| CN113667841A (en) * | 2021-07-14 | 2021-11-19 | 四川省冕宁县方兴稀土有限公司 | Method for extracting rare earth and recovering fluorine resource from bastnaesite |
| CN114348983A (en) * | 2022-01-12 | 2022-04-15 | 四川省乐山锐丰冶金有限公司 | Method for producing rare earth chloride and co-producing iron phosphate by using mangting parabastnaesite |
| CN114480835A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN115637340A (en) * | 2022-11-03 | 2023-01-24 | 东北大学 | System for converting and cleanly leaching suspension-state mineral phase of mixed rare earth concentrate and using method thereof |
| CN115874068A (en) * | 2022-11-03 | 2023-03-31 | 东北大学 | Method for mixed rare earth concentrate ore phase transformation-clean leaching |
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Cited By (18)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105803187A (en) * | 2016-05-19 | 2016-07-27 | 东北大学 | Microwave-assisted decomposition method for Baotou mixed rare earth concentrates |
| CN106801153A (en) * | 2016-12-30 | 2017-06-06 | 包头稀土研究院 | A kind of method of low cost enrichment high-grade mixed rare earth concentrates |
| CN106916975A (en) * | 2017-03-07 | 2017-07-04 | 四川省冕宁县方兴稀土有限公司 | A kind of method of Extraction of rare earth in thorium waste residue from iron |
| CN106916975B (en) * | 2017-03-07 | 2018-08-14 | 四川省冕宁县方兴稀土有限公司 | A method of the Extraction of rare earth from iron thorium waste residue |
| 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 |
| 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 |
| CN109266838A (en) * | 2017-07-18 | 2019-01-25 | 有研稀土新材料股份有限公司 | The processing method of bastnaesite and the composite ore containing bastnaesite |
| CN110512098A (en) * | 2019-08-29 | 2019-11-29 | 包头钢铁（集团）有限责任公司 | A kind of method that bastnaesite wet process prepares rare earth chloride |
| CN111187926A (en) * | 2020-01-07 | 2020-05-22 | 包钢集团矿山研究院（有限责任公司） | Method for hydrometallurgical smelting of baiyuneboite concentrate |
| CN111636001A (en) * | 2020-05-19 | 2020-09-08 | 四川省冕宁县方兴稀土有限公司 | Acid-base combined method for treating bastnaesite and recovering rare earth from waste slag |
| CN113667841A (en) * | 2021-07-14 | 2021-11-19 | 四川省冕宁县方兴稀土有限公司 | Method for extracting rare earth and recovering fluorine resource from bastnaesite |
| CN114348983A (en) * | 2022-01-12 | 2022-04-15 | 四川省乐山锐丰冶金有限公司 | Method for producing rare earth chloride and co-producing iron phosphate by using mangting parabastnaesite |
| CN114348983B (en) * | 2022-01-12 | 2024-03-22 | 四川省乐山锐丰冶金有限公司 | Method for producing rare earth chloride and co-producing ferric phosphate by using palace bastnaesite |
| CN114480835A (en) * | 2022-01-28 | 2022-05-13 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN114480835B (en) * | 2022-01-28 | 2023-12-12 | 包头稀土研究院 | Method for decomposing mixed rare earth concentrate and use of composition |
| CN115637340A (en) * | 2022-11-03 | 2023-01-24 | 东北大学 | System for converting and cleanly leaching suspension-state mineral phase of mixed rare earth concentrate and using method thereof |
| CN115874068A (en) * | 2022-11-03 | 2023-03-31 | 东北大学 | Method for mixed rare earth concentrate ore phase transformation-clean leaching |
| CN115637340B (en) * | 2022-11-03 | 2023-09-12 | 东北大学 | Mixed rare earth concentrate suspension state ore phase conversion-clean leaching system and use method thereof |
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