CN110468275A - Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object - Google Patents
Remove the method for sulfate radical and the product obtained by this method in rare-earth precipitation object Download PDFInfo
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- CN110468275A CN110468275A CN201910922071.XA CN201910922071A CN110468275A CN 110468275 A CN110468275 A CN 110468275A CN 201910922071 A CN201910922071 A CN 201910922071A CN 110468275 A CN110468275 A CN 110468275A
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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
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
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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
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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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
A kind of method removing sulfate radical in rare-earth precipitation object is disclosed, comprising: forms solution step, pretreated rare-earth precipitation object is configured to the solution of sulphate-containing ion and rare earth ion；Settling step is added in the solution as precipitating reagent using oxalates and carries out precipitation reaction, obtains sediment；And purification step, the sediment is dissolved with hydrochloric acid, then carries out secondary precipitation by precipitating reagent of carbonate.Method of the invention effectively improves the purity of rare earth oxide；Simplify the process flow of rare-earth precipitation object purifying；Reduce energy consumption；Avoid the generation of waste residue solid waste.
Description
Technical field
The present invention relates to field of hydrometallurgy, and in particular to remove rare-earth precipitation object in sulfate radical method and by this method
Obtained product.
Background technique
Precipitating is essential purification method in metallurgy industry production, actually almost all of hydrometallurgy stream
Can all there be precipitation process in journey, it has the characteristics that easy to operate, at low cost, small investment.Precipitating be take appropriate measures make it is molten
Solute supersaturation in liquid, the method separated after being precipitated with solid forms.With the continuous improvement required product quality,
Requirement to the impurity content in sediment is also continuously improved.In Extraction of rare earth element, rare earth element and impurity element are realized
Efficiently separate and have great importance.The separation of rare earth element and non-rare earth impurity can be divided into crude separation and purification two
Point, purification is except trace impurity from Rare Earth Elements Determination, and high purity rare earth oxide is produced frequently with oxalate precipitation
Method and extraction etc. refine rare earth oxide.And commonly use sulfuric acid in extracting rare-earth element technical process and carry out extraction reaction,
A large amount of sulfate ion can be introduced into enter in reaction system, and after depositing technology, sulfate radical can be with corresponding rare earth
Element and precipitating reagent form double salt, have seriously affected the degree of purity of rare earth oxide.
A large amount of sulfate ion can be contained in the rare-earth precipitation object prepared at present, seriously reduce the pure of rare-earth substance
Degree, influences the quality of rare-earth substance.For the sulfate radical in removal rare earth object, each Rare Earth Factory can remove sulphur therein using barium chloride
Acid ion will cause certain problem.Poisonous and harmful substance barium chloride is introduced first in precipitating, secondly, can generate big
The secondary residue barium sulfate of amount.Meanwhile needing to improve calcination process temperature to improve rare-earth precipitation object purity, cause to prepare rare earth
The energy consumption of substance improves, to seriously constrain the effective use and exploitation of rare-earth substance.
Summary of the invention
In order to overcome drawbacks described above, the present invention provides in a kind of removing rare-earth precipitation object the method for sulfate radical and by this method
Product obtained.
The present invention provides a kind of method for removing sulfate radical in rare-earth precipitation object, comprising: forms solution step, will pre-process
Rare-earth precipitation object be configured to the solution of sulphate-containing ion and rare earth ion；Settling step is added by precipitating reagent of oxalates
Precipitation reaction is carried out into the solution, obtains sediment；And purification step, the sediment is dissolved with hydrochloric acid, then with
Carbonate is that precipitating reagent carries out secondary precipitation.
Another embodiment according to the present invention, in the formation solution step, sulfate ion concentration in the solution
For 0.50~1.5mol/l, preferably 0.75~1.5mol/l.
Another embodiment according to the present invention, in the settling step, before the precipitating reagent is added further include:
The solution is heated to 70~100 DEG C, preferably 75~95 DEG C；Dispersing agent is added with into the solution.
Another embodiment according to the present invention, in the settling step, with the molar ratio of rare earth ion and oxalates
Precipitating reagent is added into the solution for 1:1~1:5, at the same add pH adjuster make pH value of reaction system maintain 1.0~
Between 3.0, preferably 1.5~3；And be kept stirring, mixing speed is 100~300r/min, preferably 100~200r/min；
It persistently being stirred after having added the precipitating reagent, the speed of the stirring is 50~200r/min, preferably 100~150r/min,
Mixing time is 15~90min, preferably 30~90min.
Another embodiment according to the present invention further includes the first aging step after the settling step, described old
Change 70~100 DEG C of temperature, preferably 75~95 DEG C；The digestion time is 30~200min, preferably 60~180min.
Another embodiment according to the present invention, in the purification step, with rare earth ion and hydrochloric acid molar ratio for 1:
1.5~1:4 addition hydrochloric acid is dissolved, preferably 1:2~1:3；Heating temperature is 20~70 DEG C, preferably 30~50 DEG C；It stirs
It is 100~300r/min that mix speed, which be mixing speed, preferably 100~200r/min；Mixing time is 15~90min, preferably
For 30~90min.
Another embodiment according to the present invention is with rare earth ion and carbonate molar ratio in the purification step
1:2~1:6 adds carbonate.
Another embodiment according to the present invention further includes the second aging step after the purification step, described old
Change 70~100 DEG C of temperature, preferably 75~95 DEG C；The digestion time is 30~200min, preferably 60~180min.
Another embodiment according to the present invention, described in 700~1100 DEG C of maturing temperature range, preferably 800~
1000℃；Calcining time is 100~400min, preferably 120~300min.
The present invention also provides a kind of earth oxide products as made from the above method.
Method of the invention carries out precipitation process using oxalates as rare-earth precipitation agent, to containing earth solution, passes through
Filter processing obtains object containing rare-earth precipitation；A certain amount of dissolving with hydrochloric acid will be added in above-mentioned rare-earth precipitation object and form rare earth-iron-boron, make
Secondary precipitation reaction is carried out with carbonate deposition agent, obtains rare-earth precipitation object by filtration treatment, is obtained by calcination process pure
Net rare earth oxide.Method of the invention effectively improves the purity of rare earth oxide；Simplify the purifying of rare-earth precipitation object
Process flow；Reduce energy consumption；Avoid the generation of waste residue solid waste.
Detailed description of the invention
Its example embodiment is described in detail by referring to accompanying drawing, above and other feature of the invention and advantage will become
It is more obvious.
Fig. 1 is the flow diagram of method of the invention.
Specific embodiment
It elaborates With reference to embodiment to the present invention.
As shown in Figure 1, the method for removing sulfate radical in rare-earth precipitation object of the invention, comprising: S1 forms solution step, will
Pretreated rare-earth precipitation object is configured to the solution of sulphate-containing ion and rare earth ion；S2 settling step is heavy with oxalates
Shallow lake agent, which is added in the solution, carries out precipitation reaction, obtains sediment；And S3 purification step, it is with hydrochloric acid that the sediment is molten
Then solution carries out secondary precipitation by precipitating reagent of carbonate.
" pretreated rare-earth precipitation object " described in this patent refers to the solid matter including sulfate radical and rare earth element.
In S1 step, in the solution sulfate ion concentration be 0.50~1.5mol/l, preferably 0.75~
1.5mol/l。
It in S2 step, is added before precipitating reagent to accelerate to react, solution can be heated and improve reaction temperature.Solution
Temperature is preferably kept at 70~100 DEG C, more preferably 75~95 DEG C.In order to increase the dispersibility of sediment, ammonium salt can be added
Dispersing agent, while maintain system pH between 1.0~3.0.It later, is 1:1 with the molar ratio of rare earth ion and oxalates
~1:5 adds oxalic acid precipitation agent into solution.Persistently addition alkaline ph values regulator makes pH value of reaction system maintain 1.0 simultaneously
Between~3.0, preferably 1.5~3.And be kept stirring, mixing speed is 100~300r/min, preferably 100~200r/
min.It is persistently stirred after having added precipitating reagent, the speed of stirring is 50~200r/min, preferably 100~150r/min, stirring
Time is 15~90min, preferably 30~90min.
It further include the first aging step, 70~100 DEG C of Aging Temperature, preferably 75~95 DEG C after S2 step；Ageing
Time is 30~200min, preferably 60~180min.
The solution obtained after ageing is filtered processing later and obtains sediment.Water can be used and ethyl alcohol repeats respectively
Washing precipitate for several times, to remove impurity.Then in the S3 step, using the filtered sediment of hydrochloric acid solution.With rare earth from
Son is 1:1.5~1:4, the preferably ratio of 1:2~1:3 with hydrochloric acid molar ratio, and hydrochloric acid is added and is dissolved.It is anti-in order to accelerate
It answers, it is 20~70 DEG C, preferably 30~50 DEG C that temperature can be heated to system.Meanwhile system can be stirred, it stirs
Speed is that mixing speed is 100~300r/min, preferably 100~200r/min.Mixing time is 15~90min, preferably
30~90min.
Another embodiment according to the present invention further includes the first aging step after the settling step, described old
Change 70~100 DEG C of temperature, preferably 75~95 DEG C；The digestion time is 30~200min, preferably 60~180min.
After hydrochloric acid is reacted with sediment completion, carbonate, such as sodium carbonate sodium, potassium carbonate etc. are added into system, into
Row secondary precipitation.Carbonate is added with rare earth ion and carbonate molar ratio for 1:2~1:6.
It further include the second aging step, 70~100 DEG C of Aging Temperature, preferably 75~95 DEG C after secondary precipitation.It is old
The change time is 30~200min, preferably 60~180min.
The solution obtained after ageing is filtered processing later and obtains sediment.Water can be used and ethyl alcohol repeats respectively
Washing precipitate for several times, to remove impurity.And it is to obtain purer rare earth that sediment is dried under the conditions of 70~120 DEG C of temperature
Sediment powder body material.
Rare-earth precipitation powder material being roasted later, such as in Muffle kiln roasting, maturing temperature is 700 DEG C~
1100 DEG C, calcining time is preferably 100~400min, and sample cools to room temperature with the furnace later, obtains purer rare-earth oxidation
Powder material.
Embodiment 1
It is 0.75mol/l containing earth solution that pretreated rare-earth precipitation object, which is configured to sulfate radical content,.In 80 DEG C of items
Under part, a certain amount of ammonium sulfate dispersing agent is added, under the stirring condition of 100r/min, according to rare earth ion and precipitating reagent mole
Than constantly adding oxalate precipitation agent into reactor for 1:2, the pH value of ammonium salt adjustment system is during which continued on simultaneously, is made anti-
The pH value of system is answered to maintain 1.5 or so.After having added precipitating reagent, it is ensured that the final pH value of system be 1.5 or so, then with
The mixing speed of 100r/min persistently stirs 30min, after reaction ageing reaction 60min under the conditions of 80 DEG C of temperature.It will obtain
It obtains precipitation system and carries out suction filtration processing, during which wash 3 times and 5 times respectively using water and ethyl alcohol.It will be dilute using a certain amount of hydrochloric acid
The dissolution of native deposit sample, rare-earth precipitation object is placed in precipitation reactor, adds the pure water of 100ml for chloride containing rare earth mother solution
Dilution.Under the conditions of 30 DEG C of temperature, under condition of normal pressure, under the stirring condition of 100r/min, one is added into precipitation reactor
Quantitative Ammonium bicarbonate food grade precipitating reagent, causes former rare earth ion and carbonate molar ratio ratio is 1:3.Ammonium bicarbonate precipitation agent is added
Afterwards, 30min is stirred persistently with the mixing speed of 100r/min, ageing reaction 60min under the conditions of 30 DEG C of temperature.By containing for acquisition
The solution system of rare-earth precipitation sample carries out suction filtration processing, is during which washed respectively 3 and 5 times using water and ethyl alcohol, and by acquisition
Sample is placed in drying box, dries 300min under the conditions of 100 DEG C.Sample after drying and processing is placed in corundum crucible
In, calcination process 300min under the conditions of 800 DEG C in Muffle furnace, sample cools to room temperature, the rare-earth oxidation of acquisition with the furnace later
Object show that wherein sulfur content is about 1.57% by analysis.
Embodiment 2
It is 1.5mol/l containing earth solution that pretreated rare-earth precipitation object, which is configured to sulfate radical content,.In 95 DEG C of conditions
Under, a certain amount of ammonium sulfate dispersing agent is added, under the stirring condition of 200r/min, according to rare earth ion and precipitating reagent molar ratio
Oxalate precipitation agent is constantly added into reactor for 1:2, is during which continued on the pH value of ammonium salt adjustment system simultaneously, is made to react
The pH value of system maintains 3 or so.After having added precipitating reagent, it is ensured that the final pH value of system is 3 or so, then with 100r/min
Mixing speed persistently stir 90min, after reaction under the conditions of 95 DEG C of temperature ageing reaction 180min.Body is precipitated by obtaining
System carries out suction filtration processing, during which washs 3 times and 5 times respectively using water and ethyl alcohol.Using a certain amount of hydrochloric acid by rare-earth precipitation sample
Product dissolution, rare-earth precipitation object is placed in precipitation reactor, the pure water for adding 100ml dilutes chloride containing rare earth mother solution.In
Under the conditions of 60 DEG C of temperature, under condition of normal pressure, under the stirring condition of 200r/min, a certain amount of carbon is added into precipitation reactor
Sour sodium precipitating reagent, causes former rare earth ion concentration and carbonate molar ratio is 1:4.After having added sodium carbonate precipitating reagent, with 100r/
The mixing speed of min persistently stirs 90min, ageing reaction 180min under the conditions of 60 DEG C of temperature.Acquisition is contained into rare-earth precipitation
The solution system of sample carries out suction filtration processing, is during which washed respectively 3 and 5 times using water and ethyl alcohol, and the sample of acquisition is placed
In drying box, 300min is dried under the conditions of 110 DEG C.Sample after drying and processing is placed in corundum crucible, in Muffle
Calcination process 200min under the conditions of 900 DEG C in furnace, sample cools to room temperature with the furnace later, and the rare earth oxide of acquisition is by analysis
It obtains, wherein sulfur content is about 0.12%.
Embodiment 3
It is 1.0mol/l containing earth solution that pretreated rare-earth precipitation object, which is configured to sulfate radical content,.In 75 DEG C of conditions
Under, a certain amount of ammonium sulfate dispersing agent is added, under the stirring condition of 200r/min, according to rare earth ion and precipitating reagent molar ratio
Oxalate precipitation agent is constantly added into reactor for 1:2, is during which continued on the pH value of ammonium salt adjustment system simultaneously, is made to react
The pH value of system maintains 2 or so.After having added precipitating reagent, it is ensured that the final pH value of system is 2 or so, then with 100r/min
Mixing speed persistently stir 90min, after reaction under the conditions of 75 DEG C of temperature ageing reaction 90min.Body is precipitated by obtaining
System carries out suction filtration processing, during which washs 3 times and 5 times respectively using water and ethyl alcohol.Using a certain amount of hydrochloric acid by rare-earth precipitation sample
Product dissolution, rare-earth precipitation object is placed in precipitation reactor, the pure water for adding 100ml dilutes chloride containing rare earth mother solution.In
Under the conditions of 50 DEG C of temperature, under condition of normal pressure, under the stirring condition of 200r/min, a certain amount of carbon is added into precipitation reactor
Sour ammonium precipitant solution, causes former rare earth ion concentration and hydroxide concentration ratio is 1:3.After having added precipitating reagent, with 100r/
The mixing speed of min persistently stirs 90min, ageing reaction 90min under the conditions of 50 DEG C of temperature.By the sample containing rare-earth precipitation of acquisition
The solution system of product carries out suction filtration processing, is during which washed respectively 3 and 5 times using water and ethyl alcohol, and the sample of acquisition is placed in
In drying box, 420min is dried under the conditions of 100 DEG C.Sample after drying and processing is placed in corundum crucible, in Muffle furnace
In calcination process 120min under the conditions of 1000 DEG C, sample cools to room temperature with the furnace later, and the rare earth oxide of acquisition is by analysis
It obtains, wherein sulfur content is about 0.63%.
Comparative example 1
It is 0.75mol/l containing earth solution that pretreated rare-earth precipitation object, which is configured to sulfate radical content,.In 80 DEG C of items
Under part, a certain amount of ammonium sulfate dispersing agent is added, under the stirring condition of 100r/min, according to rare earth ion and precipitating reagent mole
Than constantly adding oxalate precipitation agent into reactor for 1:2, the pH value of ammonium salt adjustment system is during which continued on simultaneously, is made anti-
The pH value of system is answered to maintain 1.5 or so.After having added precipitating reagent, it is ensured that the final pH value of system be 2 or so, then with
The mixing speed of 100r/min persistently stirs 30min, after reaction ageing reaction 60min under the conditions of 80 DEG C of temperature.It will obtain
It obtains precipitation system and carries out suction filtration processing, during which wash 3 times and 5 times respectively using water and ethyl alcohol.The sample of acquisition is placed in dry
In dry case, 420min is dried under the conditions of 80 DEG C.Sample after drying and processing is placed in corundum crucible, in Muffle furnace
Calcination process 300min under the conditions of 800 DEG C, sample cools to room temperature with the furnace later, and the rare earth oxide of acquisition obtains by analysis
Out, wherein sulfur content is about 5.33%.
The result of comparative example 1-3 and comparative example 1, it can be seen that it is dilute that pretreatment can be significantly reduced in method of the invention
Sulfate radical content in native sediment improves the purity of earth oxide product.
Present invention disclosed above preferred embodiment is only intended to help to illustrate the present invention.There is no detailed for preferred embodiment
All details are described, are not limited the invention to the specific embodiments described.Obviously, according to the content of this specification,
It can make many modifications and variations.These embodiments are chosen and specifically described to this specification, is in order to better explain the present invention
Principle and practical application, so that skilled artisan be enable to better understand and utilize the present invention.The present invention is only
It is limited by claims and its full scope and equivalent.
Claims (10)
1. a kind of method for removing sulfate radical in rare-earth precipitation object, comprising:
Solution step is formed, pretreated rare-earth precipitation object is configured to the solution of sulphate-containing ion and rare earth ion；
Settling step is added in the solution as precipitating reagent using oxalates and carries out precipitation reaction, obtains sediment；And
Purification step is dissolved the sediment with hydrochloric acid, then carries out secondary precipitation by precipitating reagent of carbonate.
2. the method according to claim 1, wherein in the formation solution step, sulfate radical in the solution
Ion concentration is 0.50~1.5mol/l, preferably 0.75~1.5mol/l.
3. the method according to claim 1, wherein in the settling step, be added the precipitating reagent it
Before further include:
The solution is heated to 70~100 DEG C, preferably 75~95 DEG C；With
Dispersing agent is added into the solution.
4. the method according to claim 1, wherein in the settling step, with rare earth ion and oxalates
Molar ratio be that 1:1~1:5 adds precipitating reagent into the solution, while adding pH adjuster maintains pH value of reaction system
Between 1.0~3.0, preferably 1.5~3；And be kept stirring, mixing speed be 100~300r/min, preferably 100~
200r/min；It persistently being stirred after having added the precipitating reagent, the speed of the stirring is 50~200r/min, preferably 100~
150r/min, mixing time are 15~90min, preferably 30~90min.
5. the method according to claim 1, wherein further including the first ageing step after the settling step
Suddenly, 70~100 DEG C of the Aging Temperature, preferably 75~95 DEG C；The digestion time be 30~200min, preferably 60~
180min。
6. the method according to claim 1, wherein being rubbed in the purification step with rare earth ion and hydrochloric acid
You are than being that 1:1.5~1:4 carbon skeleton hydrochloric acid is dissolved, preferably 1:2~1:3；Heating temperature be 20~70 DEG C, preferably 30~
50℃；Mixing speed is that mixing speed is 100~300r/min, preferably 100~200r/min；Mixing time be 15~
90min, preferably 30~90min.
7. the method according to claim 1, wherein in the purification step, with rare earth ion and carbonate
Molar ratio is that 1:2~1:6 adds carbonate.
8. the method according to claim 1, wherein further including the second ageing step after the purification step
Suddenly, 70~100 DEG C of the Aging Temperature, preferably 75~95 DEG C；The digestion time be 30~200min, preferably 60~
180min。
9. according to the method described in claim 8,700~1100 DEG C of maturing temperature range described in it is characterized in that, preferably
800~1000 DEG C；Calcining time is 100~400min, preferably 120~300min.
10. a kind of earth oxide product, which is characterized in that be made by method described in claim 1-9.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662866A (en) * | 2020-12-16 | 2021-04-16 | 江西理工大学 | Method for reducing sulfate radical content in rare earth oxide by carbonization roasting |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112662866A (en) * | 2020-12-16 | 2021-04-16 | 江西理工大学 | Method for reducing sulfate radical content in rare earth oxide by carbonization roasting |
| CN112662866B (en) * | 2020-12-16 | 2022-04-01 | 江西理工大学 | Method for reducing sulfate radical content in rare earth oxide by carbonization roasting |
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