CN110144456A - The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt - Google Patents
The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt Download PDFInfo
- Publication number
- CN110144456A CN110144456A CN201910534197.XA CN201910534197A CN110144456A CN 110144456 A CN110144456 A CN 110144456A CN 201910534197 A CN201910534197 A CN 201910534197A CN 110144456 A CN110144456 A CN 110144456A
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- China
- Prior art keywords
- calcium
- rare earth
- calcium chloride
- calcium salt
- ion type
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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
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- 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
-
- 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 technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt the invention discloses a kind of, it uses calcium compound for raw material, calcium chloride solution is produced for leaching ion type rareearth, can not only sulphur ammonium be replaced to solve the problems, such as ammonia and nitrogen pollution, simultaneously, because of calcium compound abundant raw material and cheap, its cost of made calcium chloride solution is significantly less than the raw materials such as sulphur ammonium, magnesium sulfate, aluminum sulfate, so as to reduce the cost of winning of ion type rareearth, good economic benefit and social benefit are realized.
Description
Technical field
The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt the present invention relates to a kind of.
Technical background
Sulphur ammonium multi-purpose greatly makees leaching agent to the exploitation of south China ion type rareearth at present, due to using ammonium salt in production,
The ammonia and nitrogen pollution to surrounding enviroment can be generated.To solve this problem, in recent years many technological staffs be respectively adopted sodium sulphate,
The non-ammonium salt leaching agent such as magnesium sulfate, aluminum sulfate leaches ion type rareearth, and has carried out a large amount of research and Practical experiments work, takes
Obtained certain achievement.But using these raw materials to make, leaching agent cost is higher, and some is even also higher than sulphur ammonium, promotes and applies
It has certain problems.For reduce ion type rareearth cost of winning, there is an urgent need to develop new inexpensive leaching agent, realize from
Subtype rare earth mining low cost, lasting exploit.
Summary of the invention
That it is an object of the invention to provide a kind of production costs is low, environmental pollution is small produces chlorination with dissolving with hydrochloric acid calcium salt
The technique that calcium directly leaches ion type rareearth.
Of the invention produces the technique that calcium chloride directly leaches ion type rareearth, including following step with dissolving with hydrochloric acid calcium salt
It is rapid:
1, it measures the content of effective calcium in calcium salt: taking a certain amount of calcium salt, such as calcium oxide, calcium hydroxide, calcium carbonate, measuring it has
Imitate the content of ingredient；
2, calcium powder is produced: the calcium salt powder of granularity required for calcium salt is made；
3, calcium salt is sized mixing: the calcium salt powder produced being added in reactor, water purification is added, slurries are made in stirring；
4, leaching liquid calcium chloride is produced: according to the percentage composition of the amount of taken calcium salt and contained effective calcium component, needed for calculating
Hydrochloric acid is added in calcium salt slurries the amount of hydrochloric acid (technical hydrochloric acid), stirring while adding, until the reaction is complete, it is molten that calcium chloride is made
Liquid；
5, rare earth leaching liquid is prepared: after calcium chloride solution percentage concentration made of measuring, by calcium chloride concentration needed for leaching rare earth
Water purification is added to be configured to ion type rareearth leaching agent；
6, rare earth leaches: by selected ion type rareearth raw ore, measuring its rare earth grade, calculates contained in the rare-earth original ore
Rare earth content (REO amount), by rare earth (REO): calcium chloride (quality)=1:1-50 calculates the amount of required leaching agent, controls speed
In degree injection raw ore, calcium ion is sufficiently exchanged with rare-earth original ore, forms rare earth mother solution；
7, rare earth mother solution cleans: in the rare earth mother solution that previous step obtains plus adjusting PH with base value 5-5.4 is clarified, and is made in mother liquor
AL3+、Fe3+Ion forms hydroxide precipitating and removes；
8, rare-earth precipitation: being slowly added to calcium hydroxide slurry in the mother liquor that previous step has cleaned, and it is small to be aged 24 when being added
When, then filters pressing (or natural filtration) obtains the rare earth hydrate that total amount is greater than 85%.
Of the invention produces the technique that calcium chloride directly leaches ion type rareearth with dissolving with hydrochloric acid calcium salt, using calcium compound
For raw material, calcium chloride solution is produced for leaching ion type rareearth, not only sulphur ammonium can be replaced to solve the problems, such as ammonia and nitrogen pollution, together
When, because of calcium compound abundant raw material and cheap, made its cost of calcium chloride solution be significantly less than sulphur ammonium, magnesium sulfate,
The raw materials such as aluminum sulfate realize good economic benefit and social benefit so as to reduce the cost of winning of ion type rareearth.
Specific embodiment
Embodiment 1:
Using calcium oxide and technical hydrochloric acid as raw material, produce calcium chloride solution leaching ion type rareearth for.
It comprises the concrete steps that:
1, the content of free calcium oxide in calcium oxide is measured, 2000g quick lime is accurately weighed, measuring its calcium oxide content is 85%；
2, calcium powder is produced, and 2000g quick lime is crushed or Mechanical Crushing, and the pulverized limestone that granularity is 100 mesh is made；
3, calcium powder is sized mixing, and the addition of 1000g calcium powder is taken to be prepared in advance in container, and 1000g water purification stirring is added by solid-to-liquid ratio 1:1,
Slurries are made；
4, leaching liquid calcium chloride solution is produced, and according to calculating, the technical hydrochloric acid of 7386g concentration 30% is slowly added to calcium oxide slurry
In liquid, the as fully reacting as pH6-7, surveying calcium chloride concentration is about 25%；
5, rare earth leaching liquid is prepared, the calcium chloride solution for being 25% by the concentration produced, and water purification dilution is added to be configured to 3% calcium chloride
Solution；
6, rare earth leach: by 5000g rare earth grade be 0.5% ion type rareearth raw ore be packed into prepare in advance peace high 120cm,
In the leaching ore pillar of diameter 7.5cm, the rare earth calculated in 5000g rare-earth original ore is 2.5g, by rare earth: calcium chloride=1:10 ratio
The calcium chloride solution that 833ml concentration is 3% is added in raw ore column example, exchanges leaching mine agent sufficiently with the rare earth in raw ore, to
When ore leachate will have been flowed from leaching ore pillar, 1200ml water purification elution is slowly added into leaching ore pillar, after having eluted, sampling is surveyed
Mother liquor rare earth concentration is 1.5g/L, and the rare earth content calculated in re dip solution (rare earth mother solution) is 2.3g, and rare earth leaching rate is
92%；
7, rare earth mother solution cleans: in the rare earth mother solution that previous step obtains plus adjusting PH with base value 5-5.4 is clarified, and is made in mother liquor
AL3+、Fe3+Ion forms hydroxide precipitating and removes；
8, rare-earth precipitation: it is slowly added to calcium hydroxide slurry in the mother liquor that previous step has cleaned, is stirred while adding, pH is worked as
It is to precipitate completely when value is 7-7.5, is aged 24 hours, then filters pressing (natural filtration) obtains the hydroxide that total amount is greater than 85%
Rare earth.
Embodiment 2:
Using calcium hydroxide and technical hydrochloric acid as raw material, produce calcium chloride solution leaching ion type rareearth for.
It comprises the concrete steps that:
1, the content for measuring effective calcium hydroxide in calcium hydroxide, accurately weighs 1000g calcium hydroxide powder, measures its calcium hydroxide
Content be 95%；
2, calcium hydroxide is sized mixing, and 1000g calcium hydroxide powder is added in preprepared container, is added by solid-to-liquid ratio 1:1
1000g water purification, stirring, is made slurries；
3, leaching liquid calcium chloride solution is produced, and is that 30% technical hydrochloric acid is slowly added to calcium hydroxide by 3123g concentration according to calculating
In slurries, when fully reacting pH6-7, as fully reacting, surveying calcium chloride concentration is 25%；
4, leaching liquid calcium chloride solution is produced, and according to calculating, the technical hydrochloric acid of 7386g concentration 30% is slowly added to calcium oxide slurry
In liquid, the as fully reacting as pH6-7, surveying calcium chloride concentration is about 25%；
5, rare earth leaching liquid is prepared, the calcium chloride solution for being 25% by the concentration produced, and water purification dilution is added to be configured to 3% calcium chloride
Solution；
6, rare earth leach: by 5000g rare earth grade be 0.5% ion type rareearth raw ore be packed into prepare in advance peace high 120cm,
In the leaching ore pillar of diameter 7.5cm, the rare earth calculated in 5000g rare-earth original ore is 2.5g, by rare earth: calcium chloride=1:10 ratio
The calcium chloride solution that 833ml concentration is 3% is added in raw ore column example, exchanges leaching mine agent sufficiently with the rare earth in raw ore, to
When ore leachate will have been flowed from leaching ore pillar, 1200ml water purification elution is slowly added into leaching ore pillar, after having eluted, sampling is surveyed
Mother liquor rare earth concentration is 1.5g/L, and the rare earth content calculated in re dip solution (rare earth mother solution) is 2.3g, and rare earth leaching rate is
92%；
7, rare earth mother solution cleans: in the rare earth mother solution that previous step obtains plus adjusting PH with base value 5-5.4 is clarified, and is made in mother liquor
AL3+、Fe3+Ion forms hydroxide precipitating and removes；
8, rare-earth precipitation: it is slowly added to calcium hydroxide slurry in the mother liquor that previous step has cleaned, is stirred while adding, pH is worked as
It is to precipitate completely when value is 7-7.5, is aged 24 hours, then filters pressing (natural filtration) obtains the hydroxide that total amount is greater than 85%
Rare earth.
Claims (1)
1. a kind of produce the technique that calcium chloride directly leaches ion type rareearth with dissolving with hydrochloric acid calcium salt, it is characterised in that: it includes
Following steps:
(1), it measures the content of effective calcium in calcium salt: calcium salt being taken to measure the content of its effective component；
(2), calcium powder is produced: the calcium salt powder of granularity required for calcium salt is made；
(3), calcium salt is sized mixing: the calcium salt powder produced being added in reactor, water purification is added, slurries are made in stirring；
(4), leaching liquid calcium chloride is produced: according to the percentage composition of the amount of taken calcium salt and contained effective calcium component, calculating institute
Hydrochloric acid is added in calcium salt slurries the amount for needing hydrochloric acid, stirring while adding, until the reaction is complete, calcium chloride solution is made；
(5), rare earth leaching liquid is prepared: dense by calcium chloride needed for leaching rare earth after calcium chloride solution percentage concentration made of measuring
Degree plus water purification are configured to ion type rareearth leaching agent；
(6), rare earth leaches: by selected ion type rareearth raw ore, measuring its rare earth grade, calculates institute in the rare-earth original ore
The rare earth content contained, in mass ratio, rare earth: calcium chloride=1:1-50 calculates the amount of required leaching agent, injects in raw ore, calcium ion
It is sufficiently exchanged with rare-earth original ore, forms rare earth mother solution；
(7), rare earth mother solution cleans: in the rare earth mother solution that previous step obtains plus adjusting PH with base value 5-5.4 is clarified, and is made in mother liquor
AL3+、Fe3+Ion forms hydroxide precipitating and removes；
(8), rare-earth precipitation: being slowly added to calcium hydroxide slurry in the mother liquor that previous step has cleaned, and is aged 24 when being added
Hour, then filters pressing obtains the rare earth hydrate that total amount is greater than 85%.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201910534197.XA CN110144456A (en) | 2019-06-20 | 2019-06-20 | The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt |
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| CN201910534197.XA CN110144456A (en) | 2019-06-20 | 2019-06-20 | The technique that calcium chloride directly leaches ion type rareearth is produced with dissolving with hydrochloric acid calcium salt |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112359232A (en) * | 2020-10-14 | 2021-02-12 | 南昌华亮光电有限责任公司 | Ion adsorption type rare earth extraction method using calcium chloride as leaching agent |
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| CN102190325A (en) * | 2010-03-17 | 2011-09-21 | 北京有色金属研究总院 | Method for recovering rare earth from ionic type rare earth crude ore |
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| CN106830046A (en) * | 2017-03-07 | 2017-06-13 | 太原科技大学 | A kind of preparation method of calcium chloride solution |
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| CN1058200A (en) * | 1991-05-14 | 1992-01-29 | 齐鲁乙烯无机化工厂 | A kind of method of producing liquid calcium chloride |
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| WO2016128621A1 (en) * | 2015-02-12 | 2016-08-18 | Outotec (Finland) Oy | Method and arrangement of recovering rare earth elements from ion adsorption clays |
| CN105112692A (en) * | 2015-10-11 | 2015-12-02 | 江西理工大学 | Ore leaching method for ion-adsorbing type rare earth ore |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112359232A (en) * | 2020-10-14 | 2021-02-12 | 南昌华亮光电有限责任公司 | Ion adsorption type rare earth extraction method using calcium chloride as leaching agent |
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Application publication date: 20190820 |