CN103952554A - Method for precipitating excellent-acid-solubility cerium-containing rare-earth carbonate - Google Patents
Method for precipitating excellent-acid-solubility cerium-containing rare-earth carbonate Download PDFInfo
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- CN103952554A CN103952554A CN201410210983.1A CN201410210983A CN103952554A CN 103952554 A CN103952554 A CN 103952554A CN 201410210983 A CN201410210983 A CN 201410210983A CN 103952554 A CN103952554 A CN 103952554A
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Abstract
The invention belongs to the technical field of production of rare-earth carbonate, and particularly relates to a method for precipitating excellent-acid-solubility cerium-containing rare-earth carbonate. The method comprises the following steps: carrying out ultrasonic degassing or vacuum degassing to remove dissolved gas in a cerium-containing rare-earth solution, a precipitant solution and dilution water for solutions; while stirring, reacting the degassed precipitant solution with the cerium-containing rare-earth solution until the pH value is 6.5-7.5 so as to completely precipitate the rare earth; and dehydrating the precipitate, and washing to obtain the cerium-containing rare-earth carbonate. The acid solubility effect of the cerium-containing rare-earth carbonate is obviously improved, the solution is clear and transparent, and the turbidity is less than 5.0NTU, so the acid solubility effect is similar to that of the product precipitated by the traditional ammonium bicarbonate. The method achieves the effect of enhancing the acid solubility of the cerium-containing rare-earth carbonate, is simpler to operate, and has certain industrial popularization meanings.
Description
Technical field
The invention belongs to the production technical field of carbonated rare earth, specifically relate to a kind of method that excellent solubility in acid contains cerium carbonated rare earth that precipitates.
Background technology
Carbonated rare earth containing cerium mainly comprises cerous carbonate, Phosbloc cerium, carbonic acid La-Ce-Pr, few cerium carbonated rare earth, they are important source material of preparing the series product such as cerous nitrate, ceric ammonium nitrate, cerous sulfate, catalyzer and polishing material, conventionally cerous carbonate or Phosbloc cerium are further used after acid is molten again, so their solubility in acid is most important.In carbonated rare earth preparation, conventional precipitation agent is bicarbonate of ammonia, and the cerous carbonate being settled out or Phosbloc cerium particle are large, be easy to precipitation and washing, and solubility in acid is very good.And now under the pressure of environmental stress, avoid the pollution of ammonia nitrogen, and consider enterprise cost benefit, in the production process of cerous carbonate, start to adopt sodium carbonate as precipitation agent.But the aqueous solution of sodium carbonate, pH is higher, when it is when being combined containing cerium rare earth chloride liquid, very easily forms Ce (OH)
3and Ce (OH)
4, cause the solubility in acid of cerous carbonate or Phosbloc cerium bad, for the thorough dissolving of this type of salt is often needed, add excessive acid or add the reductive agent hydrotropies such as hydrogen peroxide, this just brings obstacle to the application of this series products, and the competitiveness of product in market is not enough.
Patent < < method > > (application number: 201210532105.2) utilize hyperacoustic cavitation effect aids precipitation carbonated rare earth that can significantly reduce the carbonated rare earth crystallisation process chlorine root amount of carrying secretly, only relate to the entrainment problem of chlorion, the solubility property containing cerium carbonated rare earth is not studied.
At present, when preparation contains cerium carbonated rare earth, for having no at present report containing the bad research of cerium carbonated rare earth solubility in acid, for adopting ultrasonic degas and the feasible way of vacuum outgas head it off also to have no report.
Summary of the invention
The object of this invention is to provide a kind of method that excellent solubility in acid contains cerium carbonated rare earth that precipitates, improved the acid soluble effect containing cerium carbonated rare earth, scientific and reasonable, simple to operate.
The excellent solubility in acid of precipitation of the present invention is containing the method for cerium carbonated rare earth, and step is as follows:
(1) adopt ultrasonic degas or vacuum outgas to remove containing dissolved gases in dilution water for cerium mischmetal feed liquid, precipitant solution and feed liquid;
(2), under the condition stirring, make precipitant solution after degassed and containing the reaction of cerium mischmetal feed liquid, terminal pH is 6.5-7.5, and rare earth is precipitated completely;
(3) precipitation is through dehydration, and washing obtains containing cerium carbonated rare earth.
The ultrasonic frequency of the ultrasonic degas described in step (1) is 25-130kHz, and ultrasonic time is 1-60min.Ultrasonic degas be ultrasonic head is inserted in solution or the tank wall of each solution on, ultrasonic 1-60min.
The vacuum tightness of the vacuum outgas described in step (1) is-1KPa ﹣-0.1MPa that the degassed time is 1-60min.Vacuum outgas is that vacuum pump is connected with pipeline with the storage tank of each solution, opens vacuum pump, controls reach-1KPa of vacuum tightness ﹣-0.1MPa, degassed 1-60min.
Described in step (1) containing cerium mischmetal feed liquid be Cerium II Chloride feed liquid, cerous nitrate feed liquid, lanthanum-cerium chloride feed liquid, lanthanum nitrate cerium feed liquid, lanthanum-cerium chloride praseodymium feed liquid, nitric acid La-Ce-Pr feed liquid, containing cerium rare earth chloride liquid or a kind of containing in cerium nitric rare earth feed liquid.
Precipitant solution described in step (1) is one or both in sodium carbonate solution or sodium hydrogen carbonate solution.
The mass percentage concentration of the precipitant solution described in step (2) is 1-20%.
The concentration containing cerium mischmetal feed liquid described in step (2) is 0.1-2.0mol/L.
Temperature of reaction described in step (2) is 5-40 ℃.
Washing time described in step (3) is 5-30min.
Washing described in step (3) adopts pure water washing, preferably adopts through sloughing the pure water of gas dissolved and washs.
In order to improve cerous carbonate, Phosbloc cerium etc. containing the solubility in acid of cerium carbonated rare earth, yield after raising acid is molten, improve the competitiveness of product in market, the present invention is by containing in the process of cerium carbonated rare earth in preparation, adopt the method for ultrasonic degas and vacuum outgas to remove preparation containing the gas dissolved in the rare earth feed liquid using in cerium carbonated rare earth, precipitant solution, dilution water, greatly reduced the amount that generates cerous hydroxide in precipitation process, after the product obtaining dissolves with acid, very as clear as crystal, performance is greatly improved.
The present invention compared with prior art, has following beneficial effect:
The molten successful of the acid containing cerium carbonated rare earth obtaining through the present invention precipitation improves, and solution is limpid bright, and its turbidity is all below 5.0NTU, and the molten effect of acid of product of traditional ammonium bicarbonate precipitation gained is very nearly the same with adopting.The present invention has reached the acid soluble effect improving containing cerium carbonated rare earth, operates relatively simply, has certain industrial dissemination.
Embodiment
Below in conjunction with embodiment, the present invention is described further.
Embodiment 1
Get the Cerium II Chloride feed liquid of Zibo Baogang glossy ganoderma rare earth extraction Workshop Production, precipitate according to the following steps successively:
(1) in the beaker of 1000ml, adding concentration is the Cerium II Chloride feed liquid 400mL of 1.35mol/L, with pure water, is diluted to 1000mL, adds the sodium carbonate solution that the concentration of having dissolved is 12% in another beaker.Adopt the method for ultrasonic degas degassed, ultrasonic frequency 40kHz, degassed 40min.
(2) under 30 ℃, the condition that stirs, sodium carbonate solution is slowly joined in Cerium II Chloride feed liquid, to supernatant liquor pH be 7.
(3), precipitation and centrifugal separation, drip washing 15min, obtains cerium carbonate product.
The cerous carbonate of preparation is dissolved in nitric acid, records its turbidity 3.2NTU.
Embodiment 2
Get the cerous nitrate feed liquid of Zibo Baogang glossy ganoderma Rare earth sealing Workshop Production, precipitate according to the following steps successively:
(1) in the filter flask of 5000ml, adding 1000mL concentration is 0.45mol/L cerous nitrate feed liquid, adds the sodium carbonate solution that the concentration of having dissolved is 10% in another filter flask.Adopt the mode of vacuumize degassing to carry out degassed, control vacuum tightness at-60KPa, degassed 15min.
(2) under 28 ℃, the condition that stirs, control sodium carbonate and cerous nitrate material feed liquid parallel-flow precipitation, the pH value of reacting after finishing is 6.8.
(3), precipitation and centrifugal separation, drip washing 10min, obtains cerium carbonate product.
The cerous carbonate of preparation is dissolved in nitric acid, records its turbidity 0.9NTU.
Embodiment 3
Get lanthanum nitrate cerium feed liquid prepared by glossy ganoderma rare earth research and development centre of Zibo Baogang, precipitate according to the following steps successively:
(1) in the filter flask of 5000ml, adding concentration is the 2000mL lanthanum nitrate cerium feed liquid of 0.86mol/L, in another filter flask, add sodium carbonate and sodium bicarbonate mixing solutions that the concentration of having dissolved is 12.5%, in the 3rd filter flask, add 4000mL pure water.Adopt the mode of vacuumize degassing to carry out degassed, control vacuum tightness at-1KPa, degassed 20min.
(2) under 5 ℃, the condition that stirs, sodium carbonate and sodium bicarbonate mixing solutions are slowly joined in lanthanum nitrate cerium feed liquid, to supernatant liquor pH be 7.
(3), precipitation and centrifugal separation, the pure water drip washing 15min with after degassed, obtains Phosbloc cerium product.
The Phosbloc cerium of preparation is dissolved in nitric acid, records its turbidity 0.85NTU.
Embodiment 4
Get Zibo Baogang glossy ganoderma rare earth extraction Workshop Production lanthanum-cerium chloride feed liquid, precipitate according to the following steps successively:
(1) in the filter flask of 5000ml, adding concentration is the 1000mL lanthanum-cerium chloride feed liquid of 0.37mol/L, adds the sodium hydrogen carbonate solution that the concentration of having dissolved is 15.1% in another filter flask, in the 3rd filter flask, adds 3000mL pure water.Adopt the mode of vacuumize degassing to carry out degassed, control vacuum tightness at-100KPa, degassed 5min.
(2) under 40 ℃, the condition that stirs, sodium hydrogen carbonate solution is slowly joined in lanthanum-cerium chloride feed liquid, to supernatant liquor pH be 7.5.
(3), precipitation and centrifugal separation, the pure water drip washing 10min with after degassed, obtains Phosbloc cerium product.
The Phosbloc cerium of preparation is dissolved in nitric acid, records its turbidity 1.5NTU.
Embodiment 5
Get Zibo Baogang glossy ganoderma rare earth extraction Workshop Production lanthanum-cerium chloride praseodymium feed liquid, precipitate according to the following steps successively:
(1) in the filter flask of 1000ml, adding concentration is the 500mL lanthanum-cerium chloride praseodymium feed liquid of 0.43mol/L, adds the sodium carbonate solution that the concentration of having dissolved is 6.7% in another filter flask, in the 3rd filter flask, adds 1000mL pure water.Adopt the mode of vacuumize degassing to carry out degassed, control vacuum tightness at-10KPa, degassed 60min.
(2) under 30 ℃, the condition that stirs, sodium carbonate solution is slowly joined in lanthanum-cerium chloride praseodymium feed liquid, to supernatant liquor pH be 7.0.
(3), precipitation and centrifugal separation, the pure water drip washing 11min with after degassed, obtains carbonic acid La-Ce-Pr product.
The carbonic acid La-Ce-Pr of preparation is dissolved in nitric acid, records its turbidity 1.7NTU.
Embodiment 6
Get nitric acid La-Ce-Pr feed liquid prepared by glossy ganoderma rare earth research and development centre of Zibo Baogang, precipitate according to the following steps successively:
(1) in the beaker of 1000ml, adding concentration is the nitric acid La-Ce-Pr feed liquid 300mL of 1.45mol/L, with pure water, is diluted to 1000mL, adds the sodium carbonate solution that the concentration of having dissolved is 12% in another beaker.Adopt the method for ultrasonic degas degassed, ultrasonic frequency 25kHz, degassed 60min.
(2) under 20 ℃, the condition that stirs, sodium carbonate solution is slowly joined in nitric acid La-Ce-Pr feed liquid, to supernatant liquor pH be 6.5.
(3), precipitation and centrifugal separation, drip washing 5min, obtains carbonic acid La-Ce-Pr product.
The carbonic acid La-Ce-Pr of preparation is dissolved in nitric acid, records its turbidity 2.2NTU.
Embodiment 7
Get Zibo Baogang glossy ganoderma rare-earth chlorination rare earth Workshop Production containing cerium rare earth chloride liquid, precipitation according to the following steps successively:
(1) in the beaker of 1000ml, add concentration be 1.85mol/L containing cerium rare earth chloride liquid 250mL, with pure water, be diluted to 1000mL, in another beaker, add the sodium carbonate solution that the concentration of having dissolved is 12%.Adopt the method for ultrasonic degas degassed, ultrasonic frequency 130kHz, degassed 1min.
(2) under 25 ℃, the condition that stirs, sodium carbonate solution is slowly joined containing in cerium rare earth chloride liquid, to supernatant liquor pH be 7.1.
(3), precipitation and centrifugal separation, drip washing 18min, obtains containing cerium carbonated rare earth product.
By being dissolved in nitric acid containing cerium carbonated rare earth of preparation, record its turbidity 2.7NTU.
Embodiment 8
Get prepared by glossy ganoderma rare earth research and development centre of Zibo Baogang containing cerium nitric rare earth feed liquid, precipitation according to the following steps successively:
(1) in the filter flask of 1000ml, add concentration be 1.35mol/L containing cerium nitric rare earth feed liquid 350mL, with pure water, be diluted to 1000mL, in another filter flask, add the sodium carbonate solution that the concentration of having dissolved is 12%.Adopt the mode of vacuumize degassing to carry out degassed, control vacuum tightness at-100KPa, degassed 1min.
(2) under 20 ℃, the condition that stirs, sodium carbonate solution is slowly joined containing in cerium nitric rare earth feed liquid, to supernatant liquor pH be 7.
(3), precipitation and centrifugal separation, drip washing 30min, obtains containing cerium carbonated rare earth product.
By being dissolved in nitric acid containing cerium carbonated rare earth of preparation, record its turbidity 2.7NTU.
Claims (9)
1. the excellent solubility in acid of precipitation, containing a method for cerium carbonated rare earth, is characterized in that step is as follows:
(1) adopt ultrasonic degas or vacuum outgas to remove containing dissolved gases in dilution water for cerium mischmetal feed liquid, precipitant solution and feed liquid;
(2), under the condition stirring, make precipitant solution after degassed and containing the reaction of cerium mischmetal feed liquid, terminal pH is 6.5-7.5, and rare earth is precipitated completely;
(3) precipitation is through dehydration, and washing obtains containing cerium carbonated rare earth.
2. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the ultrasonic frequency of the ultrasonic degas described in step (1) is 25-130kHz, and ultrasonic time is 1-60min.
3. the excellent solubility in acid of precipitation according to claim 1 is containing the method for cerium carbonated rare earth, it is characterized in that the vacuum tightness of the vacuum outgas described in step (1) is-1KPa ﹣-0.1MPa, and the degassed time is 1-60min.
4. the excellent solubility in acid of precipitation according to claim 1 is containing the method for cerium carbonated rare earth, it is characterized in that described in step (1) containing cerium mischmetal feed liquid be Cerium II Chloride feed liquid, cerous nitrate feed liquid, lanthanum-cerium chloride feed liquid, lanthanum nitrate cerium feed liquid, lanthanum-cerium chloride praseodymium feed liquid, nitric acid La-Ce-Pr feed liquid, containing cerium rare earth chloride liquid or a kind of containing in cerium nitric rare earth feed liquid.
5. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the precipitant solution described in step (1) is one or both in sodium carbonate solution or sodium hydrogen carbonate solution.
6. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the mass percentage concentration of the precipitant solution described in step (2) is 1-20%.
7. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the concentration containing cerium mischmetal feed liquid described in step (2) is 0.1-2.0mol/L.
8. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the temperature of reaction described in step (2) is 5-40 ℃.
9. the excellent solubility in acid of precipitation according to claim 1, containing the method for cerium carbonated rare earth, is characterized in that the washing time described in step (3) is 5-30min.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219962A (en) * | 2015-09-30 | 2016-01-06 | 中铝广西国盛稀土开发有限公司 | A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor |
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| CN1323908A (en) * | 2001-03-20 | 2001-11-28 | 北京方正稀土科技研究所有限公司 | Optimal dissolving method of preparing rare earth fluorochloride material liquid from bastnasite concentrate |
| CN102936029A (en) * | 2012-11-30 | 2013-02-20 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for precipitating rare earth carbonate |
| CN102978398A (en) * | 2012-12-12 | 2013-03-20 | 南昌大学 | Method for obviously lowering chlorine content in process of carbonic acid rare earth crystallization |
| CN103436697A (en) * | 2013-08-15 | 2013-12-11 | 南昌大学 | Rare-earth carbonate crystallizing and precipitating method for processing aluminum-containing rare-earth feed liquid |
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2014
- 2014-05-19 CN CN201410210983.1A patent/CN103952554B/en active Active
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1323908A (en) * | 2001-03-20 | 2001-11-28 | 北京方正稀土科技研究所有限公司 | Optimal dissolving method of preparing rare earth fluorochloride material liquid from bastnasite concentrate |
| CN102936029A (en) * | 2012-11-30 | 2013-02-20 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for precipitating rare earth carbonate |
| CN102978398A (en) * | 2012-12-12 | 2013-03-20 | 南昌大学 | Method for obviously lowering chlorine content in process of carbonic acid rare earth crystallization |
| CN103436697A (en) * | 2013-08-15 | 2013-12-11 | 南昌大学 | Rare-earth carbonate crystallizing and precipitating method for processing aluminum-containing rare-earth feed liquid |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105219962A (en) * | 2015-09-30 | 2016-01-06 | 中铝广西国盛稀土开发有限公司 | A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor |
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Denomination of invention: Method for precipitating acid soluble rare earth carbonate containing cerium Effective date of registration: 20211122 Granted publication date: 20160622 Pledgee: Zibo Linzi sub branch of Bank of Qingdao Co.,Ltd. Pledgor: Zibo Baogang Lingzhi Rare Earth High-Tech Co.,Ltd. Registration number: Y2021980012895 |
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Date of cancellation: 20221026 Granted publication date: 20160622 Pledgee: Zibo Linzi sub branch of Bank of Qingdao Co.,Ltd. Pledgor: Zibo Baogang Lingzhi Rare Earth High-Tech Co.,Ltd. Registration number: Y2021980012895 |
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