CN107739854B - A method of high pure rare earth metals are extracted by rare earth phosphate rock - Google Patents
A method of high pure rare earth metals are extracted by rare earth phosphate rock Download PDFInfo
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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
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- C—CHEMISTRY; METALLURGY
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- 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
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Abstract
The present invention provides a kind of method for extracting high pure rare earth metals by rare earth phosphate rock, is related to Rare earth metal metallurgy field, comprising the following steps: A. produces rare earth oxide by rare earth phosphate rock；B. rare earth-iron-boron is produced by rare earth oxide；C. by rare earth-iron-boron high purity rare earth metal, the present invention has easy to operate, and low energy consumption, and equipment requirement is low, and process flow is short, and production process pollutes small, the high advantage of product purity.
Description
Technical field
The present invention relates to Rare earth metal metallurgy fields, and in particular to a kind of side that high pure rare earth metals are extracted by rare earth phosphate rock
Method.
Background technique
Rare earth is because having excellent magnetic, light, the electrical property that can not replace to become magnetic, luminous and laser, storage hydrogen, superconduction
Etc. the essential basic material of new and high technologies functional material, be widely used in computer, high density data storage, communication, turn
It changes, high-precision guiding, ray particle detect and the high-tech areas, such as magnetic such as record, information superhighway and national security are taken precautions against
King's NdFeB permanent magnet is widely used in VCM, motor, MRI and sound equipment etc., and high specific energy Ni-MH battery material is widely used in communication and electricity
Electrical automobile, TbDyFe giant magnetostrictive material are widely used in zero-miss guidance and satellite positioning, underwater communication, robot, valve
Accurate control etc., K2LaI5 scintillation crystal can be applied to nuclear medicine facility such as γ camera, positron emission tomography (PET) scanner.
Since the 1960s, Finland, the U.S. and the former Soviet Union are all studied while producing phosphoric acid or phosphate fertilizer from containing dilute
The method of recovering rare earth in native phosphorus ore, but due in ore apatite it is different from the association feature of rare-earth mineral, technique specific aim
It is relatively simple, and operation and cost problem, there is no mature technologies worldwide to promote and apply.
In recent years, with increasingly depleted, the hair at full speed of the new and high technologies such as information, new material of the valuable sources such as rare earth and phosphorus
Exhibition, the comprehensive utilizating research of resource are increasingly paid attention to.At present for domestic Guizhou Zhijin County Xinhua phosphorites, Anning,
The phosphorus ores such as sharp mountain and external phosphorus ore have carried out many researchs.
Summary of the invention
(1) the technical issues of solving
In view of the deficiencies of the prior art, the present invention provides it is a kind of by rare earth phosphate rock extract high pure rare earth metals method,
With easy to operate, low energy consumption, and equipment requirement is low, and process flow is short, and production process pollutes small, the high advantage of product purity.
(2) technical solution
In order to achieve the above object, the present invention is achieved by the following technical programs:
A method of high pure rare earth metals are extracted by rare earth phosphate rock, comprising the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 5-
10h after flocculant is added, stands 5-10h, draws clear liquid and is added in No. two reactors for use, then adds into No.1 reactor
Enter phosphoric acid, after being warming up to 50 DEG C of leaching reaction 5-10h, adds flocculant, stand 5-10h, draw clear liquid and be added to No. two instead
It answers in device, then calcium dihydrogen phosphate and sulfuric acid is added into No. two reactors, be warming up to 80 DEG C, depressurize suction filtration after reacting 3-5h, receive
Collecting the phosphoric acid filter liquor containing rare earth, extractant is added into the phosphoric acid filter liquor containing rare earth and is extracted, rare earth enters in extractant,
Phosphoric acid solution is recycled in liquid separation, then the extractant containing rare earth is warming up to 30-40 DEG C, and agitation and dropping oxalic acid solution is to there is solid raw
At, stop being added dropwise, after insulation reaction 10-20h, decompression is filtered, obtain rare-earth oxalate, will the rare-earth oxalate it is dry after burn
It burns, obtains rare earth oxide；
B. it is added hydrochloric acid solution into the rare earth oxide, after 70-80 DEG C of stirring dissolved clarification, adds chloride solid,
After the reaction was continued 1-2h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, and stirring is to there is solid to generate and become
Cooling after dry, powder is placed in 500-600 DEG C of sublimation apparatus by grind into powder, is reacted 5-10h, is taken out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 90-120 DEG C, time 5-10h, obtains dilute without the crystallization water
Native chloride；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing,
It is slowly heated to 400-600 DEG C, argon gas protection is passed through, is continuously heating to 800-1000 DEG C, keep the temperature 15-30min, be continuously heating to
1200-1250 DEG C, lithium metal and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
Further, flocculant is in nano polypropylene amide, nano polysilicon acid and Nano chitosan in the step A
Any one.
Further, the concentration of sulfuric acid is 70-90% in the step A.
Further, extractant is P204 extractant or P507 extractant in the step A.
Further, the concentration of oxalic acid solution described in the step A is 20-40%.
Further, the concentration of hydrochloric acid solution is 30-40% in the step B.
Further, the drying means of dry hydrogen chloride gas described in the step B are as follows: pass sequentially through hydrogen chloride dense
Sulfuric acid and sewage chlorination calcium.
(3) beneficial effect
The present invention provides a kind of methods for extracting high pure rare earth metals by rare earth phosphate rock, have the advantages that
(1) rare earth phosphate rock is subjected to second extraction with phosphoric acid, the rare earth overwhelming majority after decomposing is made to be dissolved in phosphoric acid solution
In, be added flocculant make other impurities deposition separation, efficiently separated, rare earth by extraction after plus oxalic acid solution directly at
Salt reduces reaction step, reduces costs, and the P elements in rare earth phosphate rock are enriched in recycling in phosphoric acid solution and can weigh
It is multiple to utilize, it is at low cost, it is environmentally protective.
(2) easy to operate in the preparation process of rare earth-iron-boron, the rare earth-iron-boron produced small to the corrosion of equipment
Purity is high and be free of the crystallization water, it is not easy to deliquesce, sequential reduction process will not be had an impact；Rare earth metal is extremely active, pole
Easily being acted on C, S, O, H gas, rare earth-iron-boron reduction process carries out under protection of argon gas, therefore, it is possible to prevente effectively from
Air outside reaction system enters reaction system, thus greatly reduces the content of Gases In Metals impurity, is conducive to improve dilute
The purity of earth metal.
(3) easy to operate, low energy consumption, environmentally protective, low for equipment requirements, and process flow is short, and production process pollution is small, produces
Product purity is high.
Specific embodiment
In order to make the object, technical scheme and advantages of the embodiment of the invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, instead of all the embodiments.Based on the embodiments of the present invention, those of ordinary skill in the art are not making
Every other embodiment obtained, shall fall within the protection scope of the present invention under the premise of creative work.
Embodiment 1:
A method of high pure rare earth metals are extracted by rare earth phosphate rock, comprising the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 8h,
After nano polypropylene amide is added, 8h is stood, clear liquid is drawn and is added in No. two reactors for use, then add into No.1 reactor
Enter phosphoric acid, after being warming up to 50 DEG C of leaching reaction 6h, adds nano polypropylene amide, stand 6h, draw clear liquid and be added to No. two
In reactor, then the sulfuric acid that addition calcium dihydrogen phosphate and concentration are 80% into No. two reactors, 80 DEG C are warming up to, after reacting 4h
Decompression filters, and collects the phosphoric acid filter liquor containing rare earth, and P204 extractant is added into the phosphoric acid filter liquor containing rare earth and is extracted, rare earth
It enters in P204 extractant, phosphoric acid solution is recycled in liquid separation, then the P204 extractant containing rare earth is warming up to 35 DEG C, agitation and dropping
The oxalic acid solution that concentration is 30% stops being added dropwise to there is solid generation, and after insulation reaction 15h, decompression is filtered, and obtains rare earth oxalic acid
Calcination after rare-earth oxalate drying is obtained rare earth oxide by salt；
B. concentration is added into the rare earth oxide as 35% hydrochloric acid solution, after 75 DEG C of stirring dissolved clarifications, adds chlorine
Change ammonium solid, after the reaction was continued 1.5h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, and stirring is to there is solid
Cooling after generating and drying out, powder is placed in 550 DEG C of sublimation apparatus by grind into powder, is reacted 7h, is taken out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 100 DEG C, time 7h, obtains the rare-earth chlorination without the crystallization water
Object；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing,
500 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 900 DEG C, keep the temperature 20min, be continuously heating to 1230 DEG C, metal
Lithium and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
Wherein, in step B dry hydrogen chloride gas drying means are as follows: hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 2:
A method of high pure rare earth metals are extracted by rare earth phosphate rock, comprising the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 5h,
After nano polysilicon acid is added, 10h is stood, clear liquid is drawn and is added in No. two reactors for use, then be added into No.1 reactor
Phosphoric acid adds nano polysilicon acid, stands 8h, draw clear liquid and be added to No. two reactors after being warming up to 50 DEG C of leaching reaction 6h
In, then the sulfuric acid that addition calcium dihydrogen phosphate and concentration are 75% into No. two reactors, 80 DEG C are warming up to, depressurizes pumping after reacting 4h
The phosphoric acid filter liquor containing rare earth is collected in filter, and P507 extractant is added into the phosphoric acid filter liquor containing rare earth and is extracted, rare earth enters
In P507 extractant, phosphoric acid solution is recycled in liquid separation, then the P507 extractant containing rare earth is warming up to 35 DEG C, and agitation and dropping concentration is
30% oxalic acid solution stops being added dropwise to there is solid generation, and after insulation reaction 12h, decompression is filtered, and obtains rare-earth oxalate, will
Calcination after the rare-earth oxalate is dry, obtains rare earth oxide；
B. concentration is added into the rare earth oxide as 35% hydrochloric acid solution, after 75 DEG C of stirring dissolved clarifications, adds chlorine
Change ammonium solid, after the reaction was continued 2h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, and stirring is to there is solid raw
At and after drying out, cooling, powder is placed in 600 DEG C of sublimation apparatus by grind into powder, is reacted 10h, is taken out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 110 DEG C, time 8h, obtains the rare-earth chlorination without the crystallization water
Object；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing,
450 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 900 DEG C, keep the temperature 20min, be continuously heating to 1200 DEG C, metal
Lithium and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
Wherein, in step B dry hydrogen chloride gas drying means are as follows: hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 3:
A method of high pure rare earth metals are extracted by rare earth phosphate rock, comprising the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 5h,
After Nano chitosan is added, 5h is stood, clear liquid is drawn and is added in No. two reactors for use, then phosphorus is added into No.1 reactor
Acid adds Nano chitosan, stands 5h, draw clear liquid and be added in No. two reactors after being warming up to 50 DEG C of leaching reaction 5h,
Calcium dihydrogen phosphate and concentration is added into No. two reactors again as 70% sulfuric acid, is warming up to 80 DEG C, depressurizes suction filtration after reacting 3h,
The phosphoric acid filter liquor containing rare earth is collected, P204 extractant is added into the phosphoric acid filter liquor containing rare earth and is extracted, rare earth enters
In P204 extractant, phosphoric acid solution is recycled in liquid separation, then the P204 extractant containing rare earth is warming up to 30 DEG C, and agitation and dropping concentration is
20% oxalic acid solution stops being added dropwise to there is solid generation, and after insulation reaction 10h, decompression is filtered, and obtains rare-earth oxalate, will
Calcination after the rare-earth oxalate is dry, obtains rare earth oxide；
B. concentration is added into the rare earth oxide as 40% hydrochloric acid solution, after 80 DEG C of stirring dissolved clarifications, adds chlorine
Change ammonium solid, after the reaction was continued 2h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, and stirring is to there is solid raw
At and after drying out, cooling, powder is placed in 600 DEG C of sublimation apparatus by grind into powder, is reacted 10h, is taken out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 120 DEG C, time 10h, obtains the rare earth chlorine without the crystallization water
Compound；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing,
600 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 1000 DEG C, keep the temperature 30min, be continuously heating to 1250 DEG C, metal
Lithium and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
Wherein, in step B dry hydrogen chloride gas drying means are as follows: hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 4:
A method of high pure rare earth metals are extracted by rare earth phosphate rock, comprising the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 10h,
After nano polypropylene amide is added, 10h is stood, clear liquid is drawn and is added in No. two reactors for use, then into No.1 reactor
Phosphoric acid is added, after being warming up to 50 DEG C of leaching reaction 10h, adds nano polypropylene amide, stands 10h, draw clear liquid and be added to
In No. two reactors, then the sulfuric acid that addition calcium dihydrogen phosphate and concentration are 90% into No. two reactors, 80 DEG C are warming up to, reaction
It depressurizes and filters after 5h, collect the phosphoric acid filter liquor containing rare earth, P507 extractant is added into the phosphoric acid filter liquor containing rare earth and is extracted,
Rare earth enters in P507 extractant, and phosphoric acid solution is recycled in liquid separation, then the P507 extractant containing rare earth is warming up to 40 DEG C, stirring
It is 40% oxalic acid solution to there is solid generation that concentration, which is added dropwise, stops being added dropwise, after insulation reaction 20h, decompression is filtered, and obtains rare earth
Calcination after rare-earth oxalate drying is obtained rare earth oxide by oxalates；
B. concentration is added into the rare earth oxide as 30% hydrochloric acid solution, after 70 DEG C of stirring dissolved clarifications, adds chlorine
Change ammonium solid, after the reaction was continued 1h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, and stirring is to there is solid raw
At and after drying out, cooling, powder is placed in 500 DEG C of sublimation apparatus by grind into powder, is reacted 5h, is taken out, be put into after cooling
It is heated to 90 DEG C, time 5h in closed container full of dry hydrogen chloride gas, obtains the rare earth-iron-boron without the crystallization water；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing,
400 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 800 DEG C, keep the temperature 15min, be continuously heating to 1200 DEG C, metal
Lithium and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
Wherein, in step B dry hydrogen chloride gas drying means are as follows: hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
It should be noted that, in this document, relational terms such as first and second and the like are used merely to a reality
Body or operation are distinguished with another entity or operation, are deposited without necessarily requiring or implying between these entities or operation
In any actual relationship or order or sequence.Moreover, the terms "include", "comprise" or its any other variant are intended to
Non-exclusive inclusion, so that the process, method, article or equipment including a series of elements is not only wanted including those
Element, but also including other elements that are not explicitly listed, or further include for this process, method, article or equipment
Intrinsic element.In the absence of more restrictions, the element limited by sentence "including a ...", it is not excluded that
There is also other identical elements in process, method, article or equipment including the element.
The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although with reference to the foregoing embodiments
Invention is explained in detail, those skilled in the art should understand that: it still can be to aforementioned each implementation
Technical solution documented by example is modified or equivalent replacement of some of the technical features；And these modification or
Replacement, the spirit and scope for technical solution of various embodiments of the present invention that it does not separate the essence of the corresponding technical solution.
Claims (6)
1. a kind of method for extracting high pure rare earth metals by rare earth phosphate rock, which comprises the following steps:
A. it is added to after rare earth phosphate rock being crushed in No.1 reactor and adds phosphoric acid, be warming up to 50 DEG C of leaching reaction 5-10h, add
After entering flocculant, 5-10h is stood, clear liquid is drawn and is added in No. two reactors for use, then phosphoric acid is added into No.1 reactor,
After being warming up to 50 DEG C of leaching reaction 5-10h, flocculant is added, 5-10h is stood, clear liquid is drawn and is added in No. two reactors,
Calcium dihydrogen phosphate and sulfuric acid is added into No. two reactors again, is warming up to 80 DEG C, depressurizes suction filtration after reacting 3-5h, collects and contain rare earth
Phosphoric acid filter liquor, into the phosphoric acid filter liquor containing rare earth be added extractant extracted, rare earth enters in extractant, liquid separation recycling
Phosphoric acid solution, then the extractant containing rare earth is warming up to 30-40 DEG C, agitation and dropping oxalic acid solution stops drop to there is solid generation
Add, after insulation reaction 10-20h, decompression is filtered, and obtains rare-earth oxalate, and calcination after rare-earth oxalate drying obtains dilute
Native oxide；
B. it is added hydrochloric acid solution into the rare earth oxide, after 70-80 DEG C of stirring dissolved clarification, adds chloride solid, continue
After reacting 1-2h, heating, which is concentrated into when there remains a small amount of solution, is placed in parch on electric furnace, stirs to after there is solid to generate and dry out,
Cooling, powder is placed in 500-600 DEG C of sublimation apparatus by grind into powder, is reacted 5-10h, is taken out after cooling, be put into and be full of
It is heated to 90-120 DEG C, time 5-10h in the closed container of dry hydrogen chloride gas, obtains the rare-earth chlorination without the crystallization water
Object；
C. the rare earth-iron-boron and the mixing of reducing agent lithium co-grinding are placed in reaction vessel, vacuumize degassing, slowly
It is heated to 400-600 DEG C, argon gas protection is passed through, is continuously heating to 800-1000 DEG C, keep the temperature 15-30min, be continuously heating to
1200-1250 DEG C, lithium metal and lithium chloride evaporate, and separate between slag and metal, obtain high pure rare earth metals.
2. the method for extracting high pure rare earth metals by rare earth phosphate rock as described in claim 1, which is characterized in that the step A
Middle flocculant is any one in nano polypropylene amide, nano polysilicon acid and Nano chitosan.
3. the method for extracting high pure rare earth metals by rare earth phosphate rock as described in claim 1, which is characterized in that the step A
The concentration of middle sulfuric acid is 70-90%.
4. the method for extracting high pure rare earth metals by rare earth phosphate rock as described in claim 1, which is characterized in that the step A
Middle extractant is P204 extractant or P507 extractant.
5. the method for extracting high pure rare earth metals by rare earth phosphate rock as described in claim 1, which is characterized in that the step A
Described in oxalic acid solution concentration be 20-40%.
6. the method for extracting high pure rare earth metals by rare earth phosphate rock as described in claim 1, which is characterized in that the step B
The concentration of middle hydrochloric acid solution is 30-40%.
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| CN102465210A (en) * | 2010-11-02 | 2012-05-23 | 北京有色金属研究总院 | Method for preparing high purity rare earth metal and its apparatus |
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| RU2582404C1 (en) * | 2015-02-06 | 2016-04-27 | Федеральное государственное бюджетное учреждение науки Институт физической химии и электрохимии им. А.Н. Фрумкина Российской академии наук (ИФХЭ РАН) | Method of cleaning scandium from zirconium, thorium and iron |
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| CN105803226A (en) * | 2016-03-25 | 2016-07-27 | 长沙矿冶研究院有限责任公司 | Method for extracting rare earth and aluminum from ion adsorption type rare earth ores |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102465210A (en) * | 2010-11-02 | 2012-05-23 | 北京有色金属研究总院 | Method for preparing high purity rare earth metal and its apparatus |
| CN102796888A (en) * | 2012-09-09 | 2012-11-28 | 贵州黔鸿瑞磷稀土分裂开发有限公司 | Process for extracting rare earth from phosphate concentrate |
| RU2582404C1 (en) * | 2015-02-06 | 2016-04-27 | Федеральное государственное бюджетное учреждение науки Институт физической химии и электрохимии им. А.Н. Фрумкина Российской академии наук (ИФХЭ РАН) | Method of cleaning scandium from zirconium, thorium and iron |
| CN105731513A (en) * | 2016-01-22 | 2016-07-06 | 贵州能矿织金磷化工有限公司 | Method for preparing rare earth oxide by leaching rare earth-containing phosphorite from regenerated phosphoric acid |
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