CN110422866A - The method for preparing strontium carbonate using western rare-earth tailing is climbed - Google Patents
The method for preparing strontium carbonate using western rare-earth tailing is climbed Download PDFInfo
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- CN110422866A CN110422866A CN201910854788.5A CN201910854788A CN110422866A CN 110422866 A CN110422866 A CN 110422866A CN 201910854788 A CN201910854788 A CN 201910854788A CN 110422866 A CN110422866 A CN 110422866A
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- strontium
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F11/00—Compounds of calcium, strontium, or barium
- C01F11/18—Carbonates
- C01F11/186—Strontium or barium carbonate
- C01F11/187—Strontium carbonate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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- Inorganic Chemistry (AREA)
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Abstract
The method for preparing strontium carbonate using western rare-earth tailing is climbed, weighs rare-earth tailing first, add water, stirring, add salt acid for adjusting pH value, be filtered by vacuum, wash sulfur acid strontium rare-earth tailing filter residue；Secondly, saturated sodium carbonate is added, is mixed with beating, water bath with thermostatic control heating, stirring make the strontium sulfate in tailing be fully converted into strontium carbonate, are filtered by vacuum, and washing obtains strontium carbonate crude product；Hydrochloric acid is eventually adding to bubble is no longer generated, is filtered by vacuum, washing, hypochlorous acid, which is added, to be made ferrous oxidising at ferric iron, adds concentrated ammonia liquor, vacuum filtration, washing, drying.The present invention can not only slow down the situation of celestite ore worsening shortages using the method that rare-earth tailing prepares strontium carbonate, but also can further improve the value of rare earth resources exploitation.
Description
Technical field
The invention belongs to rare-earth tailing processing technology fields, and in particular to a kind of utilization climbs western rare-earth tailing and prepares strontium carbonate
Method.
Background technique
Strontium carbonate is the white solid powder or particle of a kind of odorless, tasteless, is not only a kind of important strontium compound,
It is a kind of important Inorganic Chemicals.Currently, the alloy etc. of numerous strontium salt products, Preparation of Metallic Strontium simple substance, strontium is all with strontium carbonate
For made of Raw material processing.Since strontium carbonate has stronger absorption to X-ray and other rays, it can be applied to light extensively
Learn the manufacture of glass, such as chromoscope (cathode-ray tube of colour television set), industrial display monitor central monitoring system, display；Strontium carbonate
Can also be used for preparing magnetic material strontium ferrite, be the dedicated PTC thermistor element of production (switch starting, demagnetization, current-limiting protection,
Constant temperature warming etc.) basic powder, simultaneously can be used for the manufacture etc. of high-grade electronic ceramics, coating, purposes is related to electronics
A industry of information, chemical industry, light industry, ceramics, metallurgy, medical treatment etc. more than ten.
The ore handling capacity that Panxi Diqu rare earth selects factory annual is about 300,000 tons, and the tailing of generation is gone through at 260,000 tons or so
About 3,000,000 tons of tailing of year accumulation, some researches show that the content of strontium is higher in Panxi Diqu rare-earth tailing, even up to arrives
46.13%, and exist in the form of strontium sulfate, it is the preferable raw material for producing strontium carbonate.
Currently, the industrial production of strontium carbonate mainly passes through the method processing celestite ore of chemistry (mainly containing SrSO4) or water chestnut
Strontium mine (mainly contains SrCO3) prepare, mainly there are carbon reduction method (also referred to as grey black method or dry method), double decomposition (also referred to as directly to turn
Change method or wet process), thermal method (also referred to as roasting method), acid system, strontium nitrate method, strontium acetate method and conversion method etc..China's celestite ore money
Source reserves are few, and due to exhaustive exploitation in those early years, resource is reduced rapidly.Therefore it adopts new technology, new technology reduction raw material
Consumption makes up resource shortage, while developing and producing the strontium carbonate kind of high added value, and other of searching production strontium carbonate are former
Material already becomes the important measures that competitiveness improves in strontium carbonate manufacturing enterprise in China's.
Summary of the invention
The purpose of the present invention is to propose to a kind of methods for preparing strontium carbonate as raw material using rare-earth tailing, the production to strontium carbonate
One new way is provided, can not only slow down the shape of celestite ore worsening shortages using the method that rare-earth tailing prepares strontium carbonate
Condition, but also can further improve the value of rare earth resources exploitation.
The technical solution adopted by the present invention is that:
The method for preparing strontium carbonate using western rare-earth tailing is climbed, comprising the following steps:
Step 1: the rare-earth tailing for weighing a certain amount of 200 mesh pours into beaker, and deionized water is added, 10- is stirred at room temperature
Being slowly added to concentration after 30min into tailing solution is 6molL-1Hydrochloric acid solution continue to stir 1- until pH value of solution ≈ 1
2h, vacuum filtration, filter residue is washed with deionized three times, the rare-earth tailing filter residue of sulfur acid strontium is obtained, filtrate separately uses it for anything else；
Step 2: the Efficient Conversion agent using saturated sodium carbonate solution as strontium sulfate, according to sodium carbonate: strontium sulfate molar ratio
The rare-earth tailing filter residue of sulfur acid strontium is mixed with beating for the ratio of 1.1-1.5:1,3h-4h, solution are heated in 80 DEG C of waters bath with thermostatic control
PH ≈ 12, stirring rate 200-300r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, and vacuum filtration, filter residue is washed
It washs completely, obtains strontium carbonate crude product；
Step 3: being added the hydrochloric acid of 6mol/L into strontium carbonate crude product again, until bubble is no longer generated, pH value of solution ≈ 2,
Stirring promotes fully reacting, vacuum filtration, residue washing three times, take filtrate be added hypochlorous acid make it is ferrous oxidising at ferric iron,
Concentrated ammonia liquor control pH value of solution ≈ 5-6 is added, the hydroxide of precipitating tapping, aluminium etc. is filtered by vacuum, residue washing three times；It takes
Excessive saturated sodium carbonate solution is added in filtrate, is sufficiently stirred, and is filtered by vacuum, residue washing three times, after taking filter residue drying, crushing i.e.
The higher strontium carbonate finished product of purity can be obtained.
The beneficial effects of the present invention are:
The present invention is mainly to climb western rare-earth tailing as raw material, by strontium utilization of resources contained therein, using precipitating
Conversion method makes strontium sulfate therein be converted into industrial magnesium strontium, and the content of product strontium carbonate meets industrial carbonic acid up to 97.2%
The grade requirement of strontium.
The present invention provides a new raw material to climb strontium contained in western rare-earth tailing as raw material for the production of strontium carbonate
Available sources also utilize for the valuable element in rare-earth tailing and provide new method, while it is increasingly short also to alleviate celestite ore
Scarce situation.
Solve a large amount of tailings containing strontium and rare earth that current Panxi Diqu rare earth selects factory to generate in rare-earth original ore treatment process,
The problem of occupying large amount of land resources, and resource and environmental pressure are alleviated, this method is simple, and process conditions are easy to control, easily grasps
Make.
By climb western rare-earth tailing prepare the method for strontium carbonate, in particular to use precipitation transformation method with Panxi Diqu rare earth choosing
A large amount of tailings containing strontium and rare earth that factory generates after carrying out rare-earth original ore processing are raw material to prepare strontium carbonate.The present invention has probed into dilute
Native tailing prepares the technological parameter of strontium carbonate under different temperatures, different pH value and different stirring rates, is high-purity carbonic acid
The raw materials for production of strontium and nanoscale strontium carbonate have done Primary Study.
Detailed description of the invention
Fig. 1 climbs the process flow chart that western rare-earth tailing prepares strontium carbonate.
Specific embodiment
Embodiment 1
The rare-earth tailing for weighing a certain amount of 200 mesh pours into beaker, deionized water is added, it is backward that constant temperature stirs certain time
The hydrochloric acid solution that concentration is 6mol/L is slowly added in tailing solution, until pH value of solution ≈ 1, constant temperature stirs 4h, and vacuum pump filters,
Filtrate is discarded, filter residue is washed with deionized three times, is obtained tentatively except the tailing after the metal oxides such as de-iron, aluminium；With full
Efficient Conversion agent with sodium carbonate liquor as strontium sulfate, is added to certain mass through in just treated tailing, 60 DEG C of constant temperature
Heating water bath 4h, pH value of solution ≈ 12, stirring rate 300r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, vacuum
Pumping filter discards filtrate, residue washing three times, strontium carbonate crude product is made；The hydrochloric acid of 6mol/L is added into strontium carbonate crude product again,
Until no longer generating bubble, pH value of solution ≈ 2, stirring promotes reaction.Vacuum pump filters, and residue washing three times, takes filtrate to be added few
Hypochlorous acid is measured, the concentrated ammonia liquor of appropriate volume is added, controls pH value of solution ≈ 6, the hydroxide of precipitating tapping, aluminium and calcium, vacuum
Pumping filter, residue washing three times；It takes filtrate that excessive saturated sodium carbonate solution is added, is sufficiently stirred, vacuum pump filters, residue washing
Three times, strontium carbonate finished product is obtained after taking filter residue drying, crushing, purity is about 64.18%.
Embodiment 2
The rare-earth tailing for weighing a certain amount of 200 mesh pours into beaker, deionized water is added, it is backward that constant temperature stirs certain time
The hydrochloric acid solution that concentration is 6mol/L is slowly added in tailing solution, until pH value of solution ≈ 1, constant temperature stirs 4h, and vacuum pump filters,
Filtrate is discarded, filter residue is washed with deionized three times, is obtained tentatively except the tailing after the metal oxides such as de-iron, aluminium；With full
Efficient Conversion agent with sodium carbonate liquor as strontium sulfate, is added to certain mass through in just treated tailing, 80 DEG C of constant temperature
Heating water bath 4h, pH value of solution ≈ 10, stirring rate 300r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, vacuum
Pumping filter discards filtrate, residue washing three times, strontium carbonate crude product is made；The hydrochloric acid of 6mol/L is added into strontium carbonate crude product again,
Until no longer generating bubble, pH value of solution ≈ 2, stirring promotes reaction.Vacuum pump filters, and residue washing three times, takes filtrate to be added few
Hypochlorous acid is measured, the concentrated ammonia liquor of appropriate volume is added, controls pH value of solution ≈ 6, the hydroxide of precipitating tapping, aluminium and calcium, vacuum
Pumping filter, residue washing three times；It takes filtrate that excessive saturated sodium carbonate solution is added, is sufficiently stirred, vacuum pump filters, residue washing
Three times, strontium carbonate finished product is obtained after taking filter residue drying, crushing, purity is about 61.2%.
Embodiment 3
The rare-earth tailing for weighing a certain amount of 200 mesh pours into beaker, deionized water is added, it is backward that constant temperature stirs certain time
The hydrochloric acid solution that concentration is 6mol/L is slowly added in tailing solution, until pH value of solution ≈ 1, constant temperature stirs 4h, and vacuum pump filters,
Filtrate is discarded, filter residue is washed with deionized three times, is obtained tentatively except the tailing after the metal oxides such as de-iron, aluminium；With full
Efficient Conversion agent with sodium carbonate liquor as strontium sulfate, is added to certain mass through in just treated tailing, 80 DEG C of constant temperature
Heating water bath 4h, pH value of solution ≈ 12, stirring rate 200r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, vacuum
Pumping filter discards filtrate, residue washing three times, strontium carbonate crude product is made；The hydrochloric acid of 6mol/L is added into strontium carbonate crude product again,
Until no longer generating bubble, pH value of solution ≈ 2, stirring promotes reaction.Vacuum pump filters, and residue washing three times, takes filtrate to be added few
Hypochlorous acid is measured, the concentrated ammonia liquor of appropriate volume is added, controls pH value of solution ≈ 6, the hydroxide of precipitating tapping, aluminium and calcium, vacuum
Pumping filter, residue washing three times；It takes filtrate that excessive saturated sodium carbonate solution is added, is sufficiently stirred, vacuum pump filters, residue washing
Three times, strontium carbonate finished product is obtained after taking filter residue drying, crushing, purity is about 79.7%.
Embodiment 4
The rare-earth tailing for weighing a certain amount of 200 mesh pours into beaker, deionized water is added, it is backward that constant temperature stirs certain time
The hydrochloric acid solution that concentration is 6mol/L is slowly added in tailing solution, until pH value of solution ≈ 1, constant temperature stirs 4h, and vacuum pump filters,
Filtrate is discarded, filter residue is washed with deionized three times, is obtained tentatively except the tailing after the metal oxides such as de-iron, aluminium；With full
Efficient Conversion agent with sodium carbonate liquor as strontium sulfate, is added to certain mass through in just treated tailing, 80 DEG C of constant temperature
Heating water bath 4h, pH value of solution ≈ 12, stirring rate 300r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, vacuum
Pumping filter discards filtrate, residue washing three times, strontium carbonate crude product is made；The hydrochloric acid of 6mol/L is added into strontium carbonate crude product again,
Until no longer generating bubble, pH value of solution ≈ 2, stirring promotes reaction.Vacuum pump filters, and residue washing three times, takes filtrate to be added few
Hypochlorous acid is measured, the concentrated ammonia liquor of appropriate volume is added, controls pH value of solution ≈ 6, the hydroxide of precipitating tapping, aluminium and calcium, vacuum
Pumping filter, residue washing three times；It takes filtrate that excessive saturated sodium carbonate solution is added, is sufficiently stirred, vacuum pump filters, residue washing
Three times, strontium carbonate finished product is obtained after taking filter residue drying, crushing, purity is about 89.2%.
Claims (1)
1. using the method that western rare-earth tailing prepares strontium carbonate is climbed, which comprises the following steps:
Step 1: the rare-earth tailing for weighing 200 mesh pours into beaker, and deionized water is added, and is stirred at room temperature after 10-30min to tail
It is 6molL that concentration is slowly added in mineral solution-1Hydrochloric acid solution continue to stir 1-2h until pH value of solution ≈ 1, vacuum filtration,
Filter residue is washed with deionized three times, the rare-earth tailing filter residue of sulfur acid strontium is obtained, filtrate separately uses it for anything else；
Step 2: the Efficient Conversion agent using saturated sodium carbonate solution as strontium sulfate, according to sodium carbonate: strontium sulfate molar ratio is
The rare-earth tailing filter residue of sulfur acid strontium is mixed with beating by the ratio of 1.1-1.5:1, and 3h-4h, pH value of solution are heated in 80 DEG C of waters bath with thermostatic control
≈ 12, stirring rate 200-300r/min, make the strontium sulfate in tailing be fully converted into strontium carbonate, vacuum filtration, residue washing
Completely, strontium carbonate crude product is obtained；
Step 3: being added the hydrochloric acid of 6mol/L into strontium carbonate crude product again, until bubble is no longer generated, pH value of solution ≈ 2, stirring
Promoting fully reacting, vacuum filtration residue washing three times, takes filtrate addition hypochlorous acid to make ferrous oxidising at ferric iron, then plus
Enter concentrated ammonia liquor control pH value of solution ≈ 5-6, the hydroxide of precipitating tapping, aluminium etc. is filtered by vacuum, residue washing three times；Take filtrate
Excessive saturated sodium carbonate solution is added, is sufficiently stirred, is filtered by vacuum, residue washing three times, can be obtained after taking filter residue drying, crushing
To the higher strontium carbonate finished product of purity.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111850296A (en) * | 2020-07-16 | 2020-10-30 | 乐山盛和稀土股份有限公司 | Method for recovering and preparing high-purity strontium compound from rare earth ore |
| CN115491499A (en) * | 2022-09-22 | 2022-12-20 | 郑州大学 | Method for separating and recovering strontium from zinc anode mud |
| CN116283267A (en) * | 2023-04-04 | 2023-06-23 | 宜宾四川大学产业技术研究院 | Method for preparing rare earth composite permanent magnetic ferrite by using recycles in rare earth tailings |
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| CN105836780A (en) * | 2016-03-28 | 2016-08-10 | 余国礼 | Method of converting celestite into strontium carbonate under cavitation effect |
| CN110042231A (en) * | 2019-05-27 | 2019-07-23 | 中国地质科学院矿产综合利用研究所 | Method for leaching strontium from strontium-containing sulfate concentrate solid calcium |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111850296A (en) * | 2020-07-16 | 2020-10-30 | 乐山盛和稀土股份有限公司 | Method for recovering and preparing high-purity strontium compound from rare earth ore |
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| CN115491499A (en) * | 2022-09-22 | 2022-12-20 | 郑州大学 | Method for separating and recovering strontium from zinc anode mud |
| CN115491499B (en) * | 2022-09-22 | 2024-02-23 | 郑州大学 | Method for separating and recovering strontium from zinc anode slime |
| CN116283267A (en) * | 2023-04-04 | 2023-06-23 | 宜宾四川大学产业技术研究院 | Method for preparing rare earth composite permanent magnetic ferrite by using recycles in rare earth tailings |
| CN116283267B (en) * | 2023-04-04 | 2024-06-04 | 宜宾四川大学产业技术研究院 | Method for preparing rare earth composite permanent magnetic ferrite by using recycles in rare earth tailings |
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Application publication date: 20191108 |