CN107298457A - A kind of method that utilization carbon dioxide prepares rare earth carbonate - Google Patents
A kind of method that utilization carbon dioxide prepares rare earth carbonate Download PDFInfo
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- CN107298457A CN107298457A CN201710521207.7A CN201710521207A CN107298457A CN 107298457 A CN107298457 A CN 107298457A CN 201710521207 A CN201710521207 A CN 201710521207A CN 107298457 A CN107298457 A CN 107298457A
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- carbon dioxide
- rare earth
- rare
- earth carbonate
- organic matter
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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
- C01F17/00—Compounds of rare earth metals
- C01F17/20—Compounds containing only rare earth metals as the metal element
- C01F17/247—Carbonates
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- Inorganic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a kind of method that utilization carbon dioxide prepares rare earth carbonate, belong to the preparation method field of rare earth carbonate.Aim to provide a kind of without to rare earth ion progress alkali transition, directly being realized by process meanses and the method that carbon dioxide prepares rare earth carbonate being passed through under normality.Technical solutions according to the invention comprise the steps successively:Step 1:Volume ratio is equal to 1~5:1 organic matter:Soluble rare-earth salt is respectively added in reactor, and with stirring;Step 2:Carbon dioxide is passed through into reactor, rare-earth precipitation thing is obtained;Step 3:It is static, make rare-earth precipitation thing, water, organic matter layering, successively discharge rare-earth precipitation thing, water;Step 4:By rare-earth precipitation thing in Vacuum filtration device cyclic washing, suction filtration, obtain rare earth carbonate.The present invention is used for the preparation of rare earth carbonate.
Description
Technical field
It is especially a kind of to prepare rare earth carbonic acid using carbon dioxide the present invention relates to the preparation method field of rare earth carbonate
The method of salt.
Background technology
Carbonate is important industrial chemicals, is widely used in the works such as chemical industry, glass, soap, papermaking, weaving and food
Industry.Carbonate is also the important intermediate product of chemical industry synthesis, can be used for preparing metal oxide.The carbonic acid of most metals
Salt is water insoluble, thus industrially can the method for precipitation by metal ion with carbonate by way of by precipitation by metallic ion
Get off and realize separation, sediment is again that can obtain metal oxide by high temperature sintering.
The preparation method of carbonate is more, including ammonia-soda process, Alkali absorption carbon dioxide process, soluble carbonate salt precipitation indissoluble
Carbonate method, the acid carbonate thermal decomposition precipitation method.These methods have the shortcomings that it is different, such as ammonia-soda process need largely use
Ammonia alkali, cost are high, and are discharged with ammonia nitrogen, cause environmental pollution;Other several methods are required to using different precipitating reagents or added
Heat, cost is high, and has more brine waste to produce.
Carbon dioxide wide material sources, including fuel combustion, carbonate decomposition, animals and plants breathing can all produce carbon dioxide,
Wherein the carbon dioxide wide material sources of industrial fuel burning and carbonate decomposition generation, collection are simple, can be subject to Collection utilization,
Especially with the preparation process of the metal carbonate in commercial synthesis.
The content of the invention
For above-mentioned deficiency, the present invention is intended to provide a kind of method that utilization carbon dioxide prepares rare earth carbonate, the party
Method directly realizes that carbon dioxide is passed through under normality realizes carbonate by process meanses without carrying out alkali transition to rare earth ion
Prepare, technique is simple and easy to get, and cost is low, with preferably application value.
In order to realize above-mentioned technique effect, the technical scheme that the present invention is provided is such:One kind utilizes carbon dioxide system
The method of standby rare earth carbonate, comprises the steps successively:
Step 1:Volume ratio is equal to 1~5:1 organic matter:Soluble rare-earth salt is respectively added in reactor, and companion
With stirring;
Step 2:Carbon dioxide is passed through into reactor, rare-earth precipitation thing is obtained;
Step 3:It is static, make rare-earth precipitation thing, water, organic matter layering, successively discharge rare-earth precipitation thing, water;
Step 4:By rare-earth precipitation thing in Vacuum filtration device cyclic washing, suction filtration, obtain rare earth carbonate.
Preferably, the intake of the carbon dioxide described in step 2 and the mol ratio of rare-earth salts are equal to 1.65~2:1.
Preferably, described organic matter is the one or more in Ammonia organic matter, Ammonia mixing organic matter.
Preferably, described reactor is the container with sealing structure.
Preferably, the washing described in step 3 is one or more in water, alkaline aqueous solution with agent.
Preferably, the reaction pressure of step 1~4 is 0~0.2MPa.
Preferably, the mixing speed described in step 1 is 50-100r/min.
Preferably, the quiescent time described in step 3 is 30~60min.
Preferably, the suction filtration number of times described in step 4 is 3~6 times.
Preferably, also include after step 4:Cleaning solution is added into the reactor containing organic matter, 30~50min is stirred,
Water-oil separating, repeated washing 1~2 time obtains the organic matter of regeneration.
The present invention is compared with conventional method, with advantages below:
1. process exploitation Ammonia organic matter and solvable rare earth salt blend, the technique of carbon dioxide precipitates, ingenious utilization
The principle that Ammonia in acid condition extracts acid keeps system to maintain neutral level, carbon dioxide precipitates is carried out, real
Existing, solvable rare-earth salts makes the transition without alkali, and cost is low, environmentally friendly.
2. the Ammonia organic matter selected by the technique can realize back extraction regeneration under neutral system, enable organic matter real
Now recycle.
3rd, the rare earth carbonate obtained by the present invention prepares the oxide of the rare earth by high temperature sintering, and its calcination process is produced
Carbon dioxide may be recovered, realization is recycled.
Embodiment
Claims of the present invention is described in further detail with reference to embodiment, but not constituted pair
Any limitation of the present invention, any limited number of time modification made in the claims of the present invention, still in the present invention
Claims scope of the claimed in.
Embodiment 1:
Ammonia organic matter and soluble rare-earth salt volume ratio are pressed 1:1 ratio is respectively added in reactor, and with stirring
Mix;Under air-proof condition, by soluble rare-earth salt:Carbon dioxide=1:The ratio of 1.65 (mol ratios) is passed through two into reactor
Carbon oxide gas, obtain rare earth carbonate precipitation;Static 30 minutes, make rare-earth precipitation thing, water, organic matter layering;Successively by rare earth
Sediment, water are discharged in Vacuum filtration device from reactor bottom valve;Organic matter retains in a kettle.;Rare-earth precipitation thing
Pure water cyclic washing, suction filtration are used in Vacuum filtration device 3 times, obtain pure rare earth carbonate.After water-oil separating, Xiang Han
Pure water or alkaline aqueous solution are added in the reactor of organic matter, the addition of cleaning solution is the 1/3 of organic matter, persistently stirs 30 points
Clock, carries out water-oil separating after terminating, repeated washing 1 time obtains the organic matter of regeneration, for next round reaction.
Embodiment 2:
Ammonia organic matter and soluble rare-earth salt volume ratio are pressed 3:1 ratio is respectively added in reactor, and with stirring
Mix;Under air-proof condition, by soluble rare-earth salt:Carbon dioxide=1:The ratio of 1.8 (mol ratios) is passed through two into reactor
Carbon oxide gas, obtain rare earth carbonate precipitation;Static 40 minutes, make rare-earth precipitation thing, water, organic matter layering;Successively by rare earth
Sediment, water are discharged in Vacuum filtration device from reactor bottom valve;Organic matter retains in a kettle.;Rare-earth precipitation thing
Pure water cyclic washing, suction filtration are used in Vacuum filtration device 5 times, obtain pure rare earth carbonate.After water-oil separating, Xiang Han
Pure water or alkaline aqueous solution are added in the reactor of organic matter, the addition of cleaning solution is the 1/2 of organic matter, persistently stirs 50 points
Clock, carries out water-oil separating after terminating, repeated washing 2 times obtains the organic matter of regeneration, for next round reaction.
Embodiment 3:
Ammonia organic matter and soluble rare-earth salt volume ratio are pressed 5:1 ratio is respectively added in reactor, and with stirring
Mix;Under air-proof condition, by soluble rare-earth salt:Carbon dioxide=1:The ratio of 2 (mol ratios) is passed through dioxy into reactor
Change carbon gas, obtain rare earth carbonate precipitation;Static 60 minutes, make rare-earth precipitation thing, water, organic matter layering;Rare earth is sunk successively
Starch, water are discharged in Vacuum filtration device from reactor bottom valve;Organic matter retains in a kettle.;Rare-earth precipitation thing exists
Pure water cyclic washing, suction filtration are used in Vacuum filtration device 6 times, obtain pure rare earth carbonate.After water-oil separating, to containing
Pure water or alkaline aqueous solution are added in the reactor of machine thing, the addition of cleaning solution is the 1/3 of organic matter, persistently stirs 50 points
Clock, carries out water-oil separating after terminating, repeated washing 2 times obtains the organic matter of regeneration, for next round reaction.
Above-described is only presently preferred embodiments of the present invention, all timess done in the range of the spirit and principles in the present invention
What modifications, equivalent substitutions and improvements etc., should be included within the scope of the present invention.
Claims (10)
1. a kind of method that utilization carbon dioxide prepares rare earth carbonate, it is characterised in that comprise the steps successively:
Step 1:It is 1~5 by volume ratio:1 organic matter:Soluble rare-earth salt is respectively added in reactor, and with stirring;
Step 2:Carbon dioxide is passed through into reactor, rare-earth precipitation thing is obtained;
Step 3:Stand, make rare-earth precipitation thing, water, organic matter layering;
Step 4:By rare-earth precipitation thing in Vacuum filtration device cyclic washing, suction filtration, obtain rare earth carbonate.
2. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
The intake of carbon dioxide described in 2 and the mol ratio of rare-earth salts are equal to 1.65~2:1.
3. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that described
Organic matter be Ammonia organic matter, Ammonia mixing organic matter in one or more.
4. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that described
Reactor be the container with sealing structure.
5. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
Washing described in 3 is with the one or more that agent is in water, alkaline aqueous solution.
6. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that its is anti-
It is 0~0.2MPa to answer pressure.
7. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
Mixing speed described in 1 is 50~100r/min.
8. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
Quiescent time described in 3 is 30~60min.
9. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
Suction filtration number of times described in 4 is 3~6 times.
10. the method that a kind of utilization carbon dioxide according to claim 1 prepares rare earth carbonate, it is characterised in that step
Also include after rapid 4:Cleaning solution is added into the reactor containing organic matter, 30~50min, water-oil separating, repeated washing 1 is stirred
~2 times, the organic matter of regeneration is obtained, for next round reaction.
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Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109721055A (en) * | 2018-12-25 | 2019-05-07 | 武汉工程大学 | A kind of preparation method of carbonate not soluble in water |
Citations (4)
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US3374069A (en) * | 1967-03-16 | 1968-03-19 | Atomic Energy Commission Usa | Preparation of metal carbonates by co2-pressurizing anhydrous metal acetates |
CN101787438A (en) * | 2009-01-23 | 2010-07-28 | 胡建康 | Method for precipitating rare earth by adopting carbon dioxide |
CN102816930A (en) * | 2012-08-13 | 2012-12-12 | 南昌大学 | Method for gas phase precipitation of rare earth |
CN104117682A (en) * | 2013-04-27 | 2014-10-29 | 北京有色金属研究总院 | Method for preparing narrow range rare earth oxide with controllable particle size |
-
2017
- 2017-06-30 CN CN201710521207.7A patent/CN107298457A/en active Pending
Patent Citations (4)
Publication number | Priority date | Publication date | Assignee | Title |
---|---|---|---|---|
US3374069A (en) * | 1967-03-16 | 1968-03-19 | Atomic Energy Commission Usa | Preparation of metal carbonates by co2-pressurizing anhydrous metal acetates |
CN101787438A (en) * | 2009-01-23 | 2010-07-28 | 胡建康 | Method for precipitating rare earth by adopting carbon dioxide |
CN102816930A (en) * | 2012-08-13 | 2012-12-12 | 南昌大学 | Method for gas phase precipitation of rare earth |
CN104117682A (en) * | 2013-04-27 | 2014-10-29 | 北京有色金属研究总院 | Method for preparing narrow range rare earth oxide with controllable particle size |
Cited By (1)
Publication number | Priority date | Publication date | Assignee | Title |
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CN109721055A (en) * | 2018-12-25 | 2019-05-07 | 武汉工程大学 | A kind of preparation method of carbonate not soluble in water |
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