CN107739854A - A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock - Google Patents
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock Download PDFInfo
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- CN107739854A CN107739854A CN201710984203.2A CN201710984203A CN107739854A CN 107739854 A CN107739854 A CN 107739854A CN 201710984203 A CN201710984203 A CN 201710984203A CN 107739854 A CN107739854 A CN 107739854A
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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
- 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
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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
- 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 present invention provides a kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, is related to Rare earth metal metallurgy field, comprises the following steps：A. rare earth oxide is produced 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 the advantages of simple to operate, energy consumption is low, and equipment requirement is low, and technological process is short, and production process pollution is small, and product purity is high.
Description
Technical field
The present invention relates to Rare earth metal metallurgy field, and in particular to a kind of side that high pure rare earth metals are extracted by rare earth phosphate rock
Method.
Background technology
Rare earth is because becoming magnetic, luminous and laser, storage hydrogen, superconduction with excellent magnetic, light, the electrical property that can not substitute
The basic material essential etc. new and high technology functional material, be widely used in computer, high density data storage, communication, turn
Change, high accuracy 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 magnets are widely used in VCM, motor, MRI and sound equipment etc., and high specific energy Ni-MH battery materials are widely used in communication and electricity
Electrical automobile, TbDyFe giant magnetostrictive materials are widely used in zero-miss guidance and satellite fix, underwater communication, robot, valve
Accurate control etc., K2LaI5 scintillation crystals can be applied to nuclear medicine facility such as γ cameras, positron emission tomography (PET) scanner.
Since the 1960s, Finland, the U.S. and the former Soviet Union are all studied while phosphoric acid or phosphate fertilizer is produced 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 Problems, not ripe technology worldwide popularization and application.
In recent years, with the hair at full speed of the new and high technology such as the increasingly depleted of the valuable sources such as rare earth and phosphorus, information, new material
Exhibition, the comprehensive utilizating research of resource are increasingly paid attention to.Currently for domestic Guizhou Zhijin County Xinhua phosphorites, Anning,
The phosphorus ores such as sharp mountain and external phosphorus ore have carried out many researchs.
The content of the invention
(1) technical problem solved
In view of the shortcomings of the prior art, the invention provides it is a kind of by rare earth phosphate rock extract high pure rare earth metals method,
With the advantages of simple to operate, energy consumption is low, and equipment requirement is low, and technological process is short, and production process pollution is small, and product purity is high.
(2) technical scheme
To realize object above, the present invention is achieved by the following technical programs：
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, comprises the following steps：
A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 5-
10h, add flocculant after, stand 5-10h, draw clear liquid be added to it is stand-by in No. two reactors, then into No.1 reactor plus
Enter phosphoric acid, after being warming up to 50 DEG C of leaching reaction 5-10h, add flocculant, stand 5-10h, draw clear liquid and be added to No. two instead
Answer in device, then calcium dihydrogen phosphate and sulfuric acid are 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 is entered in extractant,
Phosphoric acid solution is reclaimed in liquid separation, then the extractant containing rare earth is warming up into 30-40 DEG C, and agitation and dropping oxalic acid solution is to there is solid life
Into, stop being added dropwise, after insulation reaction 10-20h, decompression filters, and obtains rare-earth oxalate, will the rare-earth oxalate dry after burn
Burn, obtain rare earth oxide；
B. hydrochloric acid solution is added into the rare earth oxide, after 70-80 DEG C is stirred dissolved clarification, adds chloride solid,
Continue after reacting 1-2h, heating is concentrated into when there remains a small amount of solution and is placed in parch on electric furnace, and stirring is to there is solid to generate and become
After dry, cooling, grind into powder, powder is placed in 500-600 DEG C of sublimation apparatus, reacts 5-10h, take 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, obtain dilute without the crystallization water
Native chloride；
C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing,
400-600 DEG C is slowly heated to, argon gas protection is passed through, is continuously heating to 800-1000 DEG C, be incubated 15-30min, be continuously heating to
1200-1250 DEG C, lithium metal evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
Further, flocculant is in nano polypropylene acid amides, 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 extractants or P507 extractants 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 is described in the step B：Hydrogen chloride is passed sequentially through dense
Sulfuric acid and sewage chlorination calcium.
(3) beneficial effect
The invention provides a kind of method that high pure rare earth metals are extracted 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 decomposition is dissolved in phosphoric acid solution
In, add flocculant make other impurities deposition separation, efficiently separated, rare earth after extraction plus oxalic acid solution directly into
Salt, reactions steps are reduced, reduce cost, and the P elements in rare earth phosphate rock are enriched in recovery in phosphoric acid solution and can weighed
Multiple to utilize, cost is low, green.
(2) easy to operate in the preparation process of rare earth-iron-boron, the corrosion to equipment is small, the rare earth-iron-boron produced
Purity is high and is free of the crystallization water, it is not easy to deliquescence, 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 is carried out under argon gas protection, therefore, it is possible to prevente effectively from
Air outside reaction system enters reaction system, so as to greatly reduce the content of Gases In Metals impurity, is advantageous to improve dilute
The purity of earth metal.
(3) simple to operate, energy consumption is low, green, low for equipment requirements, and technological process is short, and production process pollution is small, production
Product purity is high.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention,
Technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is the present invention one
Divide embodiment, rather than whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art are not making
The every other embodiment obtained under the premise of creative work, belongs to the scope of protection of the invention.
Embodiment 1：
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, comprises the following steps：
A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 8h,
Add nano polypropylene acid amides after, stand 8h, draw clear liquid be added to it is stand-by in No. two reactors, then into No.1 reactor plus
Enter phosphoric acid, after being warming up to 50 DEG C of leaching reaction 6h, add nano polypropylene acid amides, stand 6h, draw clear liquid and be added to No. two
In reactor, then calcium dihydrogen phosphate and concentration are added as 80% sulfuric acid into No. two reactors, 80 DEG C are warming up to, after reacting 4h
Decompression is filtered, and collects the phosphoric acid filter liquor containing rare earth, and P204 extractants are added into the phosphoric acid filter liquor containing rare earth and are extracted, rare earth
Enter in P204 extractants, liquid separation recovery phosphoric acid solution, then the P204 extractants containing rare earth are 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 filters, and obtains rare earth oxalic acid
Salt, calcination after the rare-earth oxalate is dried, obtains rare earth oxide；
B. the hydrochloric acid solution that concentration is 35% is added into the rare earth oxide, after 75 DEG C are stirred dissolved clarifications, adds chlorine
Change ammonium solid, continue after reacting 1.5h, heating is concentrated into when there remains a small amount of solution and is placed in parch on electric furnace, and stirring is to there is solid
After generation and exsiccation, cooling, grind into powder, powder is placed in 550 DEG C of sublimation apparatus, reacts 7h, take out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 100 DEG C, time 7h, obtain the rare-earth chlorination without the crystallization water
Thing；
C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing,
500 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 900 DEG C, be incubated 20min, be continuously heating to 1230 DEG C, metal
Lithium evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
Wherein, the drying means of dry hydrogen chloride gas is in step B：Hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 2：
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, comprises the following steps：
A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 5h,
After adding nano polysilicon acid, 10h is stood, clear liquid is drawn and is added to stand-by in No. two reactors, then added into No.1 reactor
Phosphoric acid, after being warming up to 50 DEG C of leaching reaction 6h, nano polysilicon acid is added, stands 8h, clear liquid is drawn and is added to No. two reactors
In, then calcium dihydrogen phosphate and concentration are added as 75% sulfuric acid into No. two reactors, 80 DEG C are warming up to, depressurizes and takes out after reaction 4h
Filter, collects the phosphoric acid filter liquor containing rare earth, and P507 extractants are added into the phosphoric acid filter liquor containing rare earth and are extracted, rare earth enters
In P507 extractants, liquid separation recovery phosphoric acid solution, then the P507 extractants containing rare earth are warming up to 35 DEG C, agitation and dropping concentration is
30% oxalic acid solution stops being added dropwise to there is solid generation, and after insulation reaction 12h, decompression filters, and obtains rare-earth oxalate, will
Calcination after the rare-earth oxalate is dried, obtains rare earth oxide；
B. the hydrochloric acid solution that concentration is 35% is added into the rare earth oxide, after 75 DEG C are stirred dissolved clarifications, adds chlorine
Change ammonium solid, continue after reacting 2h, heating is concentrated into when there remains a small amount of solution and is placed in parch on electric furnace, and stirring is to there is solid life
Into and be dried after, cooling, grind into powder, powder is placed in 600 DEG C of sublimation apparatus, react 10h, take out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 110 DEG C, time 8h, obtain the rare-earth chlorination without the crystallization water
Thing；
C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing,
450 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 900 DEG C, be incubated 20min, be continuously heating to 1200 DEG C, metal
Lithium evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
Wherein, the drying means of dry hydrogen chloride gas is in step B：Hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 3：
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, comprises the following steps：
A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 5h,
After adding Nano chitosan, 5h is stood, clear liquid is drawn and is added to stand-by in No. two reactors, then add phosphorus into No.1 reactor
Acid, after being warming up to 50 DEG C of leaching reaction 5h, Nano chitosan is added, stands 5h, clear liquid is drawn and is added in No. two reactors,
Calcium dihydrogen phosphate and concentration are added into No. two reactors again as 70% sulfuric acid, is warming up to 80 DEG C, suction filtration is depressurized after reacting 3h,
The phosphoric acid filter liquor containing rare earth is collected, P204 extractants are added into the phosphoric acid filter liquor containing rare earth and are extracted, rare earth enters
In P204 extractants, liquid separation recovery phosphoric acid solution, then the P204 extractants containing rare earth are warming up to 30 DEG C, agitation and dropping concentration is
20% oxalic acid solution stops being added dropwise to there is solid generation, and after insulation reaction 10h, decompression filters, and obtains rare-earth oxalate, will
Calcination after the rare-earth oxalate is dried, obtains rare earth oxide；
B. the hydrochloric acid solution that concentration is 40% is added into the rare earth oxide, after 80 DEG C are stirred dissolved clarifications, adds chlorine
Change ammonium solid, continue after reacting 2h, heating is concentrated into when there remains a small amount of solution and is placed in parch on electric furnace, and stirring is to there is solid life
Into and be dried after, cooling, grind into powder, powder is placed in 600 DEG C of sublimation apparatus, react 10h, take out, put after cooling
Enter in the closed container full of dry hydrogen chloride gas and be heated to 120 DEG C, time 10h, obtain the rare earth chlorine without the crystallization water
Compound；
C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing,
600 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 1000 DEG C, be incubated 30min, be continuously heating to 1250 DEG C, metal
Lithium evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
Wherein, the drying means of dry hydrogen chloride gas is in step B：Hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
Embodiment 4：
A kind of method that high pure rare earth metals are extracted by rare earth phosphate rock, comprises the following steps：
A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 10h,
After adding nano polypropylene acid amides, stand 10h, draw clear liquid be added to it is stand-by in No. two reactors, then into No.1 reactor
Phosphoric acid is added, after being warming up to 50 DEG C of leaching reaction 10h, nano polypropylene acid amides is added, stands 10h, draw clear liquid and be added to
In No. two reactors, then calcium dihydrogen phosphate and concentration are added as 90% sulfuric acid into No. two reactors, be warming up to 80 DEG C, reaction
Depressurize and filter after 5h, collect the phosphoric acid filter liquor containing rare earth, P507 extractants are added into the phosphoric acid filter liquor containing rare earth and are extracted,
Rare earth is entered in P507 extractants, liquid separation recovery phosphoric acid solution, then the P507 extractants containing rare earth are warming up into 40 DEG C, stirring
The oxalic acid solution that dropwise addition concentration is 40% stops being added dropwise to there is solid generation, after insulation reaction 20h, decompression suction filtration, obtains rare earth
Oxalates, calcination after the rare-earth oxalate is dried, obtains rare earth oxide；
B. the hydrochloric acid solution that concentration is 30% is added into the rare earth oxide, after 70 DEG C are stirred dissolved clarifications, adds chlorine
Change ammonium solid, continue after reacting 1h, heating is concentrated into when there remains a small amount of solution and is placed in parch on electric furnace, and stirring is to there is solid life
Into and be dried after, cooling, grind into powder, powder is placed in 500 DEG C of sublimation apparatus, react 5h, take out, be put into after cooling
90 DEG C, time 5h are heated in closed container full of dry hydrogen chloride gas, obtains the rare earth-iron-boron without the crystallization water；
C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing,
400 DEG C are slowly heated to, argon gas protection is passed through, is continuously heating to 800 DEG C, be incubated 15min, be continuously heating to 1200 DEG C, metal
Lithium evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
Wherein, the drying means of dry hydrogen chloride gas is in step B：Hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorine
Change calcium.
It should be noted that herein, such as first and second or the like relational terms are used merely to a reality
Body or operation make a distinction with another entity or operation, and not necessarily require or imply and deposited between these entities or operation
In any this actual relation or order.Moreover, term " comprising ", "comprising" or its any other variant are intended to
Nonexcludability includes, so that process, method, article or equipment including a series of elements not only will including those
Element, but also the other element including being not expressly set out, or it is this process, method, article or equipment also to include
Intrinsic key element.In the absence of more restrictions, the key element limited by sentence "including a ...", it is not excluded that
Other identical element also be present in process, method, article or equipment including the key 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
The present invention is described in detail, it will be understood by those within the art that：It still can be to foregoing each implementation
Technical scheme described in example is modified, or carries out equivalent substitution to which part technical characteristic；And these modification or
Replace, the essence of appropriate technical solution is departed from the spirit and scope of various embodiments of the present invention technical scheme.
Claims (7)
- A kind of 1. method that high pure rare earth metals are extracted by rare earth phosphate rock, it is characterised in that comprise the following steps：A. it is added to after rare earth phosphate rock is crushed in No.1 reactor and adds phosphoric acid, is warming up to 50 DEG C of leaching reaction 5-10h, adds After entering flocculant, 5-10h is stood, clear liquid is drawn and is added to stand-by in No. two reactors, then add phosphoric acid into No.1 reactor, After being warming up to 50 DEG C of leaching reaction 5-10h, flocculant is added, stands 5-10h, clear liquid is drawn and is added in No. two reactors, Calcium dihydrogen phosphate and sulfuric acid are added into No. two reactors again, is warming up to 80 DEG C, depressurizes suction filtration after reacting 3-5h, collection contains rare earth Phosphoric acid filter liquor, into the phosphoric acid filter liquor containing rare earth add extractant extracted, rare earth is entered in extractant, liquid separation recovery 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 filters, and obtains rare-earth oxalate, calcination after the rare-earth oxalate is dried, obtains dilute Native oxide；B. hydrochloric acid solution is added into the rare earth oxide, after 70-80 DEG C is stirred dissolved clarification, adds chloride solid, is continued 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 be dried, Cooling, grind into powder, powder is placed in 500-600 DEG C of sublimation apparatus, is reacted 5-10h, is taken out after cooling, be put into and be full of 90-120 DEG C, time 5-10h is heated in the closed container of dry hydrogen chloride gas, obtains the rare-earth chlorination without the crystallization water Thing；C. it is placed in after mixing the rare earth-iron-boron and reducing agent lithium co-grinding in reaction vessel, vacuumizes degassing, slowly 400-600 DEG C is heated to, argon gas protection is passed through, is continuously heating to 800-1000 DEG C, be incubated 15-30min, be continuously heating to 1200-1250 DEG C, lithium metal evaporates with lithium chloride, is separated between slag and metal, obtains high pure rare earth metals.
- 2. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step A Middle flocculant is any one in nano polypropylene acid amides, nano polysilicon acid and Nano chitosan.
- 3. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step A The concentration of middle sulfuric acid is 70-90%.
- 4. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step A Middle extractant is P204 extractants or P507 extractants.
- 5. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step A Described in the concentration of oxalic acid solution be 20-40%.
- 6. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step B The concentration of middle hydrochloric acid solution is 30-40%.
- 7. the method for high pure rare earth metals is extracted by rare earth phosphate rock as claimed in claim 1, it is characterised in that the step B Described in the drying means of dry hydrogen chloride gas be：Hydrogen chloride is passed sequentially through into the concentrated sulfuric acid and sewage chlorination calcium.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109971951A (en) * | 2019-03-31 | 2019-07-05 | 柳州呈奥科技有限公司 | A method of aluminium powder is extracted from mining site |
| CN109989074A (en) * | 2019-05-14 | 2019-07-09 | 柳州坚瑞新材料科技有限公司 | A kind of improved almag preparation method |
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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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| CN109971951A (en) * | 2019-03-31 | 2019-07-05 | 柳州呈奥科技有限公司 | A method of aluminium powder is extracted from mining site |
| CN109989074A (en) * | 2019-05-14 | 2019-07-09 | 柳州坚瑞新材料科技有限公司 | A kind of improved almag preparation method |
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| CN107739854B (en) | 2019-08-16 |
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