CN110295284A - The method for preparing solution of cerium chloride by oxidation - Google Patents
The method for preparing solution of cerium chloride by oxidation Download PDFInfo
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- CN110295284A CN110295284A CN201910744679.8A CN201910744679A CN110295284A CN 110295284 A CN110295284 A CN 110295284A CN 201910744679 A CN201910744679 A CN 201910744679A CN 110295284 A CN110295284 A CN 110295284A
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
- C22B3/24—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition by adsorption on solid substances, e.g. by extraction with solid resins
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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
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3844—Phosphonic acid, e.g. H2P(O)(OH)2
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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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- 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 discloses a kind of method for preparing solution of cerium chloride by oxidation, include the following steps: that the rare-earth chloride solution containing lanthanum chloride and cerium chloride that (1) obtains cerium praseodymium extraction and separation passes through resin column, the rare-earth chloride solution after obtaining oil removing；(2) rare-earth chloride solution after oil removing is mixed as lanthanum cerium extraction feed liquid with extractant and diluent, separates organic phase and water phase, organic phase is stripped, obtaining back extraction extraction raffinate is solution of cerium chloride by oxidation.La in the solution of cerium chloride by oxidation that the extraction yield of cerium can be improved using this method, and be prepared3+Content it is low.
Description
Technical field
The present invention relates to a kind of methods for preparing solution of cerium chloride by oxidation.
Background technique
Rare earth element is known as " industrial vitamin ", has excellent magnetic, light, the electrical property that can not replace, to improvement
Properties of product increase product variety, improve production efficiency and play the role of huge, are widely used in metallurgy, military, petroleum
The fields such as chemical industry, glass ceramics, agricultural and new material.Cerium may be used as reducing agent, catalysis as a kind of important rare earth element
Agent, alloy addition etc., and since the alloy of cerium has characteristic resistant to high temperature, it can be also used for making manufacture jet propeller zero
Part.
Ce elements are generally obtained by rare earth ore concentrate extraction and separation.In the rare-earth chloride solution be prepared by rare earth ore concentrate
A certain amount of organic impurities can be contained, organic impurities can carry under one's arms a certain amount of La3+And Ce3+.Organic impurities in rare earth-iron-boron
Enter in extraction tank with rare earth-iron-boron, is first extracted to organic phase.Since the equilibrium acidity in lanthanum cerium extraction section is lower,
The La being extracted in organic phase3+And Ce3+It is not easily accessible in the water phase of Low acid；And when carrying under one's arms La in back extraction section3+With
Ce3+Organic phase when encountering the water phase of highly acidity, the La that organic impurities is carried under one's arms3+And Ce3+It can enter in water phase, cause to be stripped
La in extraction raffinate solution of cerium chloride by oxidation3+Content increases, and the La in solution of cerium chloride by oxidation3+Content can be with the increasing of back extraction series
Add and increases.
A kind of method that programmed temperature method prepares high-pure anhydrous lanthanum chloride or cerium chloride is disclosed in CN102502757A: will
The lanthanum chloride or solution of cerium chloride by oxidation that extraction and separation are prepared from rare earth heat condensing crystallizing, obtain granular crystals；General
Bulk crystalline mixes in batch mixer with ammonium chloride by weight 4:1, is packed into porcelain bowl, porcelain bowl is uniformly put to temperature programming furnace
In, it vacuumizes, setting temperature program is begun to warm up, and is naturally cooled to 50 DEG C, is obtained anhydrous lanthanum chloride or cerium chloride, be added to water
In dissolve at once.La in the cerium chloride that this method is prepared3+Content is high.
A kind of P is disclosed in CN109680169A204The solid extracting agent of doped polyaniline and its side for extracting light rare earth
Method: using light rare earth solution as material liquid, the concentration of light rare earth is 0.01~0.1mol/L, and pH is 1~5；With polyaniline in eigenstate
With P204The ratio of solution using 5~24:1g/L are doped as solid extracting agent；By solid extracting agent and light rare earth solution with 1
Liquid-solid extraction is carried out after the ratio mixing of~5:100g/ml.This method can not be by the La in solution of cerium chloride by oxidation3+It separates, obtains
To solution of cerium chloride by oxidation in La3+Content is higher.
Summary of the invention
In view of this, the present invention provides a kind of method for preparing solution of cerium chloride by oxidation, the extraction of cerium is can be improved in this method
Rate, and La in the solution of cerium chloride by oxidation being prepared3+Content it is low.The present invention adopts the following technical scheme that realization above-mentioned purpose.
A method of solution of cerium chloride by oxidation is prepared, is included the following steps:
(1) rare-earth chloride solution containing lanthanum chloride and cerium chloride for obtaining cerium praseodymium extraction and separation passes through resin column,
Rare-earth chloride solution after obtaining oil removing；
(2) rare-earth chloride solution after oil removing is mixed as lanthanum cerium extraction feed liquid with extractant and diluent, is separated
Organic phase and water phase, organic phase is stripped, and obtaining back extraction extraction raffinate is solution of cerium chloride by oxidation；
Wherein, the cross-linked polymer formed in resin column filled with styrene and divinylbenzene.
Method in accordance with the invention it is preferred that the ratio for the cross-linked polymer that the styrene and divinylbenzene are formed
Surface area is not less than 900m2/g。
Method in accordance with the invention it is preferred that containing in the cross-linked polymer that the styrene and divinylbenzene are formed
There is the resin particle of 85%~100% partial size within the scope of 0.2~2.00mm.
Method in accordance with the invention it is preferred that the cross-linked polymer that the styrene and divinylbenzene are formed is wet
Apparent density is 0.50~0.90g/ml, and wet true density is 1.00~1.50g/ml.
Method in accordance with the invention it is preferred that the rare-earth chloride solution containing lanthanum chloride and cerium chloride passes through resin column
Flow velocity be 100~700L/h.
Method in accordance with the invention it is preferred that the rare-earth chloride solution containing lanthanum chloride and cerium chloride passes through resin column
Flow velocity be 100~600L/h.
Method in accordance with the invention it is preferred that organic impurities in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
Concentration be 5~30mg/L.
Method in accordance with the invention it is preferred that hydrogen ion is dense in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
Degree is 0.005~0.04mol/L.
Method in accordance with the invention it is preferred that rare-earth chlorination in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
The concentration of object is 0.5~4mol/L.
Method in accordance with the invention it is preferred that the ratio between the diameter of resin column and height are 1:3~20.
The present invention, which first passes through the rare-earth chloride solution containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation obtain, to fill out
The cross-linked polymer formed filled with styrene and divinylbenzene carries out oil removal treatment, and the rare-earth chloride solution after oil removing is extracted
Separation is taken, organic phase is stripped, La in obtained solution of cerium chloride by oxidation3+Content is low, and using the method increase the extractions of cerium
Rate.In currently preferred technical solution, the rare-earth chloride solution containing lanthanum chloride and cerium chloride is with 100~700L/h's
Flow velocity is by the resin column of the cross-linked polymer formed filled with styrene and divinylbenzene, the solution of cerium chloride by oxidation being prepared
In have lower La3+Content.
Specific embodiment
The present invention is further illustrated combined with specific embodiments below, but protection scope of the present invention is not limited to
This.
The method for preparing solution of cerium chloride by oxidation of the invention includes the following steps: (1) deoiling step；(2) lanthanum cerium extraction and separation
Step.
<deoiling step>
The rare-earth chloride solution containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained is obtained by resin column
Rare-earth chloride solution after oil removing.Wherein, the cross-linked polymer formed in resin column filled with styrene and divinylbenzene.
The cross-linked polymer that styrene and divinylbenzene in the present invention are formed can be obtained using conventional method.Example
Such as, styrene, divinylbenzene are obtained into the cross-linked polymeric that styrene and divinylbenzene are formed by the method for suspension polymerisation
Object.The cross-linked polymer that styrene and divinylbenzene of the invention is formed is not limited by suspension polymerisation acquisition, can also lead to
The method for crossing the routine such as polymerisation in solution, emulsion polymerization obtains.
In the present invention, the specific surface area for the cross-linked polymer that styrene and divinylbenzene are formed is not less than 900m2/g。
Preferably, the specific surface area of cross-linked polymer is not less than 1200m2/g.It is highly preferred that the specific surface area of cross-linked polymer is not less than
1500m2/g.It can achieve better deoiling effect in this way, make La in the solution of cerium chloride by oxidation being prepared3+Content it is lower, cerium
Extraction yield it is higher.
In the present invention, the wet apparent density for the cross-linked polymer that styrene and divinylbenzene are formed is 0.50~0.90g/
Ml, and wet true density is 1.00~1.50g/ml.Preferably, wet apparent density is 0.55~0.80g/ml.It is highly preferred that wet view is close
Degree is 0.65~0.75g/ml.Preferably, wet true density is 1.05~1.30g/ml.It is highly preferred that wet true density be 1.05~
1.15g/ml。
In the present invention, in the cross-linked polymer that styrene and divinylbenzene are formed, contain 85%~100% partial size
Resin particle within the scope of 0.2~2.00mm.Preferably, in the cross-linked polymer that styrene and divinylbenzene are formed, contain
There is the resin particle of 85%~100% partial size within the scope of 0.4~1.6mm.It is highly preferred that styrene and divinylbenzene shape
At cross-linked polymer in, contain 95%~100% resin particle of the partial size within the scope of 0.4~1.25mm.It in this way can be with
Reach better deoiling effect, makes La in the solution of cerium chloride by oxidation being prepared3+Content it is lower, the extraction yield of cerium is higher.
In the present invention, the diameter and height of the cross-linkable polymer resin column formed filled with styrene and divinylbenzene
The ratio between can be 1:3~20.Preferably, the ratio between the diameter of resin column and height are 1:5~15.It is highly preferred that resin column is straight
The ratio between diameter and height are 1:7~12.A specific embodiment according to the present invention, the ratio between the diameter of resin column and height are
1:10.It can achieve better deoiling effect in this way, make La in the solution of cerium chloride by oxidation being prepared3+Content it is lower, the extraction of cerium
Take rate higher.
In the present invention, the rare-earth chloride solution containing lanthanum chloride and cerium chloride that the extraction and separation of cerium praseodymium obtain passes through tree
The flow velocity of rouge column is 100~700L/h.Preferably, the rare-earth chlorination containing lanthanum chloride and cerium chloride that the extraction and separation of cerium praseodymium obtain
The flow velocity that object solution passes through resin column is 100~600L/h.It is highly preferred that cerium praseodymium extraction and separation obtain containing lanthanum chloride and chlorine
The flow velocity that the rare-earth chloride solution for changing cerium passes through resin column is 100~300L/h.It can not only guarantee the efficiency of oil removing in this way, but also
It can achieve better deoiling effect, make La in the solution of cerium chloride by oxidation being prepared3+Content it is lower, the extraction yield of cerium is higher.
Organic impurities in the present invention includes the isocyanide acyl that the collecting agent of hydroximic acid generates under high temperature or strong acid effect
Ester or amine organic compound.In rare-earth chloride solution containing lanthanum chloride and cerium chloride the concentration of organic impurities be 5~
30mg/L.Preferably, the concentration of organic impurities is 5~20mg/L in rare-earth chloride solution.It is highly preferred that rare-earth chlorination material
The concentration of organic impurities is 5~15mg/L in liquid.It can achieve better deoiling effect in this way, keep the cerium chloride being prepared molten
La in liquid3+Content it is lower, the extraction yield of cerium is higher.
In the present invention, in the rare-earth chloride solution containing lanthanum chloride and cerium chloride hydrogen ion concentration be 0.005~
0.04mol/L.Preferably, in the rare-earth chloride solution containing lanthanum chloride and cerium chloride hydrogen ion concentration be 0.005~
0.03mol/L.It is highly preferred that in the rare-earth chloride solution containing lanthanum chloride and cerium chloride hydrogen ion concentration be 0.005~
0.02mol/L。
In the present invention, the concentration of rare earth-iron-boron is 0.5 in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
~4mol/L.Preferably, in the rare-earth chloride solution containing lanthanum chloride and cerium chloride the concentration of rare earth-iron-boron be 0.5~
3mol/L.It is highly preferred that in the rare-earth chloride solution containing lanthanum chloride and cerium chloride rare earth-iron-boron concentration be 1~
3mol/L。
<lanthanum cerium extraction and separation step>
Rare-earth chloride solution after oil removing is mixed as lanthanum cerium extraction feed liquid with extractant and diluent, is separated organic
Phase and water phase, organic phase is stripped, and obtaining back extraction extraction raffinate is solution of cerium chloride by oxidation.
In the present invention, extractant used in extraction process can be acidic extractant.Preferably, acidic extractant
2- ethylhexyl phosphoric acid single 2-ethyl hexyl rouge, bis- (2- ethylhexyl) phosphates or 2- ethylhexyl phosphoric acid list 2- can be selected from
One of salt that ethylhexyl rouge is formed is a variety of.The salt that 2- ethylhexyl phosphoric acid single 2-ethyl hexyl rouge is formed can be 2-
Ethylhexyl phosphoric acid single 2-ethyl hexyl rouge ammonium salt.It is highly preferred that acidic extractant is selected from 2- ethylhexyl phosphoric acid single 2-ethyl
One of hexyl rouge, bis- (2- ethylhexyl) phosphates are a variety of.A specific embodiment according to the present invention, extraction
Agent is 2- ethylhexyl phosphoric acid single 2-ethyl hexyl rouge.
In the present invention, diluent used in extraction process is inert organic solvents.Preferably, inert organic solvents select
From one of kerosene, hexamethylene, n-hexane or a variety of.It is highly preferred that inert organic solvents are in kerosene or hexamethylene
It is one or more.A specific embodiment according to the present invention, diluent is kerosene.
In the present invention, back extraction reagent is the aqueous solution of acid.Preferably, sour aqueous solution can be the aqueous solution of hydrochloric acid
Or the aqueous solution of sulfuric acid.It is highly preferred that the aqueous solution of acid is the aqueous solution of hydrochloric acid.
In the present invention, back extraction section can carry out multistage back extraction.Preferably, 5 grades of back extraction section progress or more is stripped
It takes.It is stripped it is highly preferred that back extraction section carries out 8 grades or more.It for another example can be 12 grades for example, can be 10 grades.
The performance of styrene-divinylbenzene cross-linked polymer used in the following embodiment is referring to following table.
Table 1
Embodiment 1
Rare-earth chloride solution (the rare earth-iron-boron concentration containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained
For 1.7mol/L, hydrogen ion concentration 0.01mol/L, organic impurities concentration is 15mg/L) filling is passed through with the flow of 510L/h
(diameter 0.3m is highly 3m), after obtaining oil removing to the resin column for the cross-linked polymer for having styrene and divinylbenzene to be formed
Rare-earth chloride solution.
Feed liquid and extractant 2- ethylhexyl phosphoric acid list 2- second are extracted using the rare-earth chloride solution after oil removing as lanthanum cerium
Base hexyl rouge and diluent kerosene mixing, separate organic phase and water phase, organic phase are stripped with hydrochloric acid, is obtained more than back extraction
Liquid is solution of cerium chloride by oxidation.Calculate La in solution of cerium chloride by oxidation3+Content and cerium extraction yield, acquired results are shown in Table 2.
Embodiment 2
Rare-earth chloride solution (the rare earth-iron-boron concentration containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained
For 1.7mol/L, hydrogen ion concentration 0.01mol/L, organic impurities concentration is 10mg/L) filling is passed through with the flow of 300L/h
(diameter 0.3m is highly 3m), after obtaining oil removing to the resin column for the cross-linked polymer for having styrene and divinylbenzene to be formed
Rare-earth chloride solution.
Feed liquid and extractant 2- ethylhexyl phosphoric acid list 2- second are extracted using the rare-earth chloride solution after oil removing as lanthanum cerium
Base hexyl rouge and diluent kerosene mixing, separate organic phase and water phase, organic phase are stripped with hydrochloric acid, is obtained more than back extraction
Liquid is solution of cerium chloride by oxidation.Calculate La in solution of cerium chloride by oxidation3+Content and cerium extraction yield, acquired results are shown in Table 2.
Embodiment 3
Rare-earth chloride solution (the rare earth-iron-boron concentration containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained
For 1.7mol/L, hydrogen ion concentration 0.01mol/L, organic impurities concentration is for 8mg/L) with the flow of 600L/h by being filled with
(diameter 0.3m is highly 3m), after obtaining oil removing to the resin column for the cross-linked polymer that styrene and divinylbenzene are formed
Rare-earth chloride solution.
Feed liquid and extractant 2- ethylhexyl phosphoric acid list 2- second are extracted using the rare-earth chloride solution after oil removing as lanthanum cerium
Base hexyl rouge and diluent kerosene mixing, separate organic phase and water phase, organic phase are stripped with hydrochloric acid, is obtained more than back extraction
Liquid is solution of cerium chloride by oxidation.Calculate La in solution of cerium chloride by oxidation3+Content and cerium extraction yield, acquired results are shown in Table 2.
Embodiment 4
Rare-earth chloride solution (the rare earth-iron-boron concentration containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained
For 1.7mol/L, hydrogen ion concentration 0.01mol/L, organic impurities concentration is 20mg/L) filling is passed through with the flow of 700L/h
(diameter 0.3m is highly 3m), after obtaining oil removing to the resin column for the cross-linked polymer for having styrene and divinylbenzene to be formed
Rare-earth chloride solution.
Feed liquid and extractant 2- ethylhexyl phosphoric acid list 2- second are extracted using the rare-earth chloride solution after oil removing as lanthanum cerium
Base hexyl rouge and diluent kerosene mixing, separate organic phase and water phase, organic phase are stripped with hydrochloric acid, is obtained more than back extraction
Liquid is solution of cerium chloride by oxidation.Calculate La in solution of cerium chloride by oxidation3+Content and cerium extraction yield, acquired results are shown in Table 2.
Comparative example
Rare-earth chloride solution (the rare earth-iron-boron concentration containing lanthanum chloride and cerium chloride that cerium praseodymium extraction and separation are obtained
For 1.7mol/L, hydrogen ion concentration 0.01mol/L, organic impurities concentration is 15mg/L) as separation feed liquid and extractant 2-
Ethylhexyl phosphoric acid single 2-ethyl hexyl rouge and diluent kerosene mixing, separate organic phase and water phase, by organic phase hydrochloric acid into
Row back extraction, obtaining back extraction extraction raffinate is solution of cerium chloride by oxidation.Calculate La in solution of cerium chloride by oxidation3+Content and cerium extraction yield,
Acquired results are shown in Table 2.
Table 2
Present invention is not limited to the embodiments described above, without departing from the essence of the present invention, this field skill
Any deformation, improvement, the replacement that art personnel are contemplated that each fall within the scope of the present invention.
Claims (10)
1. a kind of method for preparing solution of cerium chloride by oxidation, which comprises the steps of:
(1) rare-earth chloride solution containing lanthanum chloride and cerium chloride for obtaining cerium praseodymium extraction and separation is obtained by resin column
Rare-earth chloride solution after oil removing；
(2) rare-earth chloride solution after oil removing is mixed as lanthanum cerium extraction feed liquid with extractant and diluent, is separated organic
Phase and water phase, organic phase is stripped, and obtaining back extraction extraction raffinate is solution of cerium chloride by oxidation；
Wherein, the cross-linked polymer formed in resin column filled with styrene and divinylbenzene.
2. the method according to claim 1, wherein the crosslinking that the styrene and divinylbenzene are formed is poly-
The specific surface area for closing object is not less than 900m2/g。
3. the method according to claim 1, wherein the crosslinking that the styrene and divinylbenzene are formed is poly-
It closes in object, contains 85%~100% resin particle of the partial size within the scope of 0.2~2.00mm.
4. the method according to claim 1, wherein the crosslinking that the styrene and divinylbenzene are formed is poly-
The wet apparent density for closing object is 0.50~0.90g/ml, and wet true density is 1.00~1.50g/ml.
5. the method according to claim 1, wherein the rare-earth chloride solution containing lanthanum chloride and cerium chloride is logical
The flow velocity for crossing resin column is 100~700L/h.
6. according to the method described in claim 5, it is characterized in that, the rare-earth chloride solution containing lanthanum chloride and cerium chloride is logical
The flow velocity for crossing resin column is 100~600L/h.
7. the method according to claim 1, wherein in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
The concentration of organic impurities is 5~30mg/L.
8. the method according to claim 1, wherein in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
Hydrogen ion concentration is 0.005~0.04mol/L.
9. the method according to claim 1, wherein in the rare-earth chloride solution containing lanthanum chloride and cerium chloride
The concentration of rare earth-iron-boron is 0.5~4mol/L.
10. any one the method according to claim 1~9, which is characterized in that the ratio between the diameter of resin column and height are 1:3
~20.
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