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 PDF

Info

Publication number
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
Authority
CN
China
Prior art keywords
carbon dioxide
rare earth
rare
earth carbonate
organic matter
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Pending
Application number
CN201710521207.7A
Other languages
Chinese (zh)
Inventor
冉俊铭
黄伟超
利天军
李剑峰
李武瑞
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
CHINALCO JINYUAN RARE-EARTH Co Ltd
Original Assignee
CHINALCO JINYUAN RARE-EARTH Co Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by CHINALCO JINYUAN RARE-EARTH Co Ltd filed Critical CHINALCO JINYUAN RARE-EARTH Co Ltd
Priority to CN201710521207.7A priority Critical patent/CN107298457A/en
Publication of CN107298457A publication Critical patent/CN107298457A/en
Pending legal-status Critical Current

Links

Classifications

    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01FCOMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
    • C01F17/00Compounds of rare earth metals
    • C01F17/20Compounds containing only rare earth metals as the metal element
    • C01F17/247Carbonates

Landscapes

  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Geology (AREA)
  • 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

A kind of method that utilization carbon dioxide prepares rare earth carbonate
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.
CN201710521207.7A 2017-06-30 2017-06-30 A kind of method that utilization carbon dioxide prepares rare earth carbonate Pending CN107298457A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201710521207.7A CN107298457A (en) 2017-06-30 2017-06-30 A kind of method that utilization carbon dioxide prepares rare earth carbonate

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201710521207.7A CN107298457A (en) 2017-06-30 2017-06-30 A kind of method that utilization carbon dioxide prepares rare earth carbonate

Publications (1)

Publication Number Publication Date
CN107298457A true CN107298457A (en) 2017-10-27

Family

ID=60135100

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201710521207.7A Pending CN107298457A (en) 2017-06-30 2017-06-30 A kind of method that utilization carbon dioxide prepares rare earth carbonate

Country Status (1)

Country Link
CN (1) CN107298457A (en)

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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)

* Cited by examiner, † Cited by third party
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

Patent Citations (4)

* Cited by examiner, † Cited by third party
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)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Similar Documents

Publication Publication Date Title
CN107089675B (en) A kind of method for the distilled ammonia wastewater recycling that ammonia-soda process soda ash is discharged
CN101648725B (en) Method for preparing industrial calcium chloride
CN108238832B (en) Method for preparing soluble potassium and calcium silicate soil conditioner by alkali-activated potassium feldspar
CN103864153B (en) PCB factory acidic etching liquid replacement extraction copper and the method preparing poly-ferric chloride
CN105566176B (en) A kind of production technology of the sour oxysome of improved 6- nitros -1,2,4
CN104018184A (en) Brand new method of producing electrolytic manganese metal
CN102275958B (en) Method for preparing magnesium hydroxide utilizing magnesium sulfate as raw material
CN104278151A (en) High-concentration-alkali-leaching comprehensive utilization process for laterite-nickel ore
CN106904647A (en) A kind of CO2Method of the mineralising with seawater resources using coupling
CN103521056A (en) Method of mineralizing and immobilizing CO2 (Carbon Dioxide) by virtue of calcium-enriched waste liquid
CN103269769A (en) Using alkaline fly ash and similar byproducts in an ion-xchange/reverse osmosis process for the production of sodium carbonate
CN102583458A (en) Method for extracting basic magnesium carbonate, iron hydroxide and calcium sulfate from serpentine under normal temperature and pressure
CN102701253B (en) CO2 mineralization method capable of co-producing potassium-enriched solution by high temperature method
CN103253689B (en) The method of lithium, magnesium is extracted from salt lake brine
CN107298457A (en) A kind of method that utilization carbon dioxide prepares rare earth carbonate
CN111099641A (en) Method for preparing high-purity lithium carbonate by extracting lithium ions
WO2013075615A1 (en) Method for joint production of potassium-rich solution by mineralizing co2
CN105779793B (en) A kind of method for separating trace uranium from bittern using coprecipitation
CN103272410B (en) In a kind of manganese sulfate electrolyte, the circularly removing technique of chlorion and cuprous hydroxide are as the application of antichlor
CN101972595A (en) Method for implementing magnesium-ammonia combined flue gas desulfuration and decarbonization and by-product recovery
CN106757119B (en) One kind is for realizing CO2The electro-chemical systems that capture is sealed up for safekeeping with mineralising
CN102671523B (en) Method for fixing light calcium carbonate as CO2 byproduct by using humate and desulfurization gypsum
CN101629250A (en) Method for reclaiming soluble manganese from electrolytic metal manganese filter-press residues
CN103130196A (en) Method for removing impurities from industrial sodium hydrosulfide
CN102351221A (en) Method for preparing magnesium hydroxide from acid-dissolved magnesium ion-containing raw materials

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
RJ01 Rejection of invention patent application after publication

Application publication date: 20171027

RJ01 Rejection of invention patent application after publication