CN101012510A - Method for hypersonic rare earth leaching - Google Patents
Method for hypersonic rare earth leaching Download PDFInfo
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- CN101012510A CN101012510A CNA2007100199443A CN200710019944A CN101012510A CN 101012510 A CN101012510 A CN 101012510A CN A2007100199443 A CNA2007100199443 A CN A2007100199443A CN 200710019944 A CN200710019944 A CN 200710019944A CN 101012510 A CN101012510 A CN 101012510A
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- leaching
- rare earth
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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- Y02P10/20—Recycling
Abstract
The invention discloses a leaching method of rare earth, which comprises the following steps: adopting sintered product of rare earth sulfuric acid as raw material and water as leaching agent; leaching through ultrasound in the ultrasonic generating device; neutralizing sediment; separating solid from liquid; setting the ultrasonic strength at 0.2-20.0W/cm2 and ultrasonic frequency at 19-80kHz.
Description
Technical field
The present invention relates to a kind of method of leaching rare earth, particularly a kind of is the method for raw material hypersonic rare earth leaching with the using rear earth ore sulfuric acid calcination products, belongs to the hydrometallurgy field.
Background technology
At present, adopting rare-earth mine sulfuric acid baking-rare earth leaching-solvent-extracted method to handle high-grade RE concentrate is the method that generally adopts in the existing Rare Earth Separation, this method is that rare earth ore concentrate and sulfuric acid are carried out roasting, change rare earth into water-soluble vitriol, leach as solvent with water then, the gained leach liquor carries out extracting and separating after neutralization, removal of impurities etc. are handled, obtain rare-earth products.The method of leaching in this method is that the using rear earth ore sulfuric acid calcination products with heat directly adds water furnishing pulpous state, squeezes into leaching vat through pump then, leaches under agitation condition.The main drawback of this leaching method that generally adopts is: the rare earth leaching efficiency is low, leaching time is long.
Summary of the invention
The objective of the invention is at the deficiencies in the prior art, a kind of method of leaching the hypersonic rare earth leaching that speed is fast, leaching efficiency is high is provided.
The technical scheme that realizes above-mentioned purpose is: a kind of method of hypersonic rare earth leaching, with the using rear earth ore sulfuric acid calcination products is raw material, with water is leaching agent, the separation and purification rare earth, it is refining that its step includes batching, leaching, neutralization precipitation, solid-liquid separation, described leaching is a supersonic leaching, and supersonic leaching is to carry out in having the supersonic leaching equipment of ultrasonic generator, and its ultrasonication intensity is 0.2～20.0W/cm
2, ultrasonic frequency is 19～80kHz.
Ultrasonication intensity when prioritization scheme of the present invention is supersonic leaching is 2.0～5.0W/cm
2, ultrasonic frequency is 19～25kHz, and the solid-to-liquid ratio of leaching using rear earth ore sulfuric acid calcination products and water is 1g: 5ml to 1g: 30ml, and service temperature is 5～60 ℃, and effect was better when service temperature was 25～40 ℃.Described supersonic leaching equipment comprises leaching container and ultrasonic generator, described leaching container is still formula or slot type or tube container, and described ultrasonic generator is any in probe type ultrasonic wave producer, vibrator type ultrasonic generator, the vibration plate formula ultrasonic generator.Supersonic leaching equipment can be that a kind of in still formula, slot type, the tube container leached a kind of the combining in container and sonde-type, vibrator type, the vibration plate formula ultrasonic generator, also can be that a kind of in still formula, slot type, the tube container leached combining of any two or three in container and sonde-type, vibrator type, the vibration plate formula ultrasonic generator.
The key of the inventive method is to have adopted supersonic leaching, ultrasonic isolating strengthening effect is mainly come from ultrasonic cavitation, ultrasonic cavitation is meant that the small complex in the liquid phase is activated under the high intense ultrasonic wave effect of low frequency, it shows as the vibration of complex, growth, a series of dynamic processes such as contraction and collapse, around cavitation bubble, produce High Temperature High Pressure in the utmost point short period of time of cavitation bubble collapse, and produce with the microjet that intensive shockwave and speed are exceedingly fast, ultrasonic cavitation produces various additive effects in microenvironment, as the turbulence effect, the perturbation effect, interfacial effect and cavity effect etc., wherein turbulence effect can make the frictional belt attenuate, increases rate of mass transfer; The perturbation effect has been strengthened the micropore diffusion; It is long-pending that interfacial effect has increased mass transfer surfaces.Therefore, ultrasonic cavitation can be strengthened the rate of mass transfer and the efficient of sepn process on the whole.Ultrasonic strengthening effect to sepn process also has heat effect and mechanical effect except cavatition.Heat effect is that molecule produces high vibration because medium absorbs ultrasonic wave and internal friction consumption, and ultransonic mechanical energy is converted into the interior energy of medium, causes that medium temperature raises.Hyperacoustic intensity is bigger, and the heat effect of generation is stronger, quickens the stripping of effective constituent, and does not change the character of composition.The propagation of ultra sonic machinery vibrational energy can form in liquid and effectively stir with mobile, pulverizes the particle in the liquid, can reach the inaccessible effect of common mechanical agitation.
After adopting technique scheme, the cavitation effect, mechanical effect and the heat effect that produce when using ultrasound ripple of the present invention is propagated in medium, strengthen dispersion, the Surface Renewal of solid-liquid interface and the material transfer between solid-liquid of solid phase in liquid phase, thereby reinforced leaching process, improved rare earth leaching process speed and efficient, leaching efficiency and speed can improve 20 to 60 times, have shortened leaching time greatly, reduce energy expenditure, and supersonic leaching process safety, reliable.
Description of drawings
Fig. 1 is a process flow diagram of the present invention;
Fig. 2～5 are several structure formations of described supersonic leaching equipment;
Fig. 2 comprises still formula container and probe type ultrasonic wave producer for probe type ultrasonic leaching still;
Fig. 3 is a vibrator type supersonic leaching groove, comprises that slot type container and several are arranged on the vibrator type ultrasonic generator on the wall of container;
Fig. 4 is a vibration plate formula supersonic leaching groove, comprises the slot type container and places the interior vibration plate formula ultrasonic generator of container;
Fig. 5 is a vibration plate formula supersonic leaching pipe, comprises tube container and places the interior vibration plate formula ultrasonic generator of container;
Among the figure: 1, probe type ultrasonic wave producer, 2, the vibrator type ultrasonic generator, 3, vibration plate formula ultrasonic generator, 4, still formula container, 5, the slot type container, 6, tube container.
Embodiment
The present invention is further detailed explanation below in conjunction with drawings and Examples.
Embodiment 1
Major equipment: stir batch mixes still, probe type ultrasonic leaching still, stir neutralization precipitation still and vacuum filtration solid-liquid separating equipment etc.
As shown in Figure 1 and Figure 2, a kind of method of hypersonic rare earth leaching is a raw material with the using rear earth ore sulfuric acid calcination products, is leaching agent with water, the separation and purification rare earth, and concrete steps are:
(1) mix: stir in the batch mixes still at 1000ml, add 450ml water, the concentrated sulfuric acid roasting material (mixed rare earth oxide content is greater than 30%) that takes by weighing the 90g rare earth ore concentrate adds in the groove type ultrasonic leaching equipment and mixes, and its solid-to-liquid ratio is 1g: 5L;
(2) supersonic leaching: in probe type ultrasonic leaching still, add the material that previous step is equipped with, carry out supersonic leaching, operational condition is ultrasonic frequency 19kHz, ultrasonication intensity 0.2W/cm
2, 5 ℃ of service temperatures behind the 35min, are closed ultra-sonic generator under ultrasonication, and the material that obtains enters next step;
(3) neutralization precipitation: in stirring the neutralization precipitation still, under agitation condition, adding neutralizing agent MgO adjusting pH value is 3-5, makes insoluble impurities separate out removal of impurities;
(4) solid-liquid separation and purification: in the vacuum filtration solid-liquid separating equipment, the previous step material is filtered, filtrate is used mishmetal concentration in the EDTA complexometric titration leach liquor, and obtaining the rare earth leaching rate is 96%, and the liquid phase filtrate that obtains further goes separation and purification to obtain rare-earth products again; Solid phase solid-liquid after washing separates, and the solid phase Separation and Recovery has valence component, and liquid phase is recyclable.
Major equipment: stir batch mixes still, vibrator type supersonic leaching groove, stir neutralization precipitation still and vacuum filtration solid-liquid separating equipment etc.
As Fig. 1, shown in Figure 3, a kind of method of hypersonic rare earth leaching is a raw material with the using rear earth ore sulfuric acid calcination products, is leaching agent with water, the separation and purification rare earth, and concrete steps are:
(1) mix: stir in the batch mixes still at 1000ml, add 900ml water, the concentrated sulfuric acid roasting material (mixed rare earth oxide content is greater than 30%) that takes by weighing the 30g rare earth ore concentrate adds in the groove type ultrasonic leaching equipment and mixes, and its solid-to-liquid ratio is 1g: 30L;
(2) supersonic leaching: in vibrator type supersonic leaching groove, add the material that previous step is equipped with, carry out supersonic leaching, operational condition is ultrasonic frequency 80kHz, ultrasonication intensity 20W/cm
2, 60 ℃ of service temperatures behind the 35min, are closed ultra-sonic generator under ultrasonication, and the material that obtains enters next step;
(3) neutralization precipitation: in stirring the neutralization precipitation still, under agitation condition, adding neutralizing agent MgO adjusting pH value is 3-5, makes insoluble impurities separate out removal of impurities;
(4) solid-liquid separation and purification: in the vacuum filtration solid-liquid separating equipment, the previous step material is filtered, filtrate is used mishmetal concentration in the EDTA complexometric titration leach liquor, and obtaining the rare earth leaching rate is 96%, and the liquid phase filtrate that obtains further goes separation and purification to obtain rare-earth products again; Solid phase solid-liquid after washing separates, and the solid phase Separation and Recovery has valence component, and liquid phase is recyclable.
Major equipment: stir batch mixes still, vibrator type supersonic leaching groove, stir neutralization precipitation still and vacuum filtration solid-liquid separating equipment etc.
As Fig. 1, shown in Figure 4, a kind of method of hypersonic rare earth leaching is a raw material with the using rear earth ore sulfuric acid calcination products, is leaching agent with water, the separation and purification rare earth, and concrete steps are:
(1) mix: stir in the batch mixes still at 1000ml, add 500ml water, the concentrated sulfuric acid roasting material (mixed rare earth oxide content is greater than 30%) that takes by weighing the 50g rare earth ore concentrate adds in the groove type ultrasonic leaching equipment and mixes, and its solid-to-liquid ratio is 1g: 10L;
(2) supersonic leaching: in vibration plate formula supersonic leaching groove, add the material that previous step is equipped with, carry out supersonic leaching, operational condition is ultrasonic frequency 25kHz, ultrasonication intensity 2W/cm
2, 40 ℃ of service temperatures behind the 35min, are closed ultra-sonic generator under ultrasonication, and the material that obtains enters next step;
(3) neutralization precipitation: in stirring the neutralization precipitation still, under agitation condition, adding neutralizing agent MgO adjusting pH value is 3-5, makes insoluble impurities separate out removal of impurities;
(4) solid-liquid separation and purification: in the vacuum filtration solid-liquid separating equipment, the previous step material is filtered, filtrate is used mishmetal concentration in the EDTA complexometric titration leach liquor, and obtaining the rare earth leaching rate is 96%, and the liquid phase filtrate that obtains further goes separation and purification to obtain rare-earth products again; Solid phase solid-liquid after washing separates, and the solid phase Separation and Recovery has valence component, and liquid phase is recyclable.
Major equipment: stir batch mixes still, vibrator type supersonic leaching groove, stir neutralization precipitation still and vacuum filtration solid-liquid separating equipment etc.
As Fig. 1, shown in Figure 5, a kind of method of hypersonic rare earth leaching is a raw material with the using rear earth ore sulfuric acid calcination products, is leaching agent with water, the separation and purification rare earth, and concrete steps are:
(1) mix: stir in the batch mixes still at 1000ml, add 450ml water, the concentrated sulfuric acid roasting material (mixed rare earth oxide content is greater than 30%) that takes by weighing the 30g rare earth ore concentrate adds in the groove type ultrasonic leaching equipment and mixes, and its solid-to-liquid ratio is 1g: 15L;
(2) supersonic leaching: in vibration plate formula supersonic leaching pipe, add the material that previous step is equipped with, carry out supersonic leaching, operational condition is ultrasonic frequency 19.8kHz, ultrasonication intensity 3W/cm
2, 30 ℃ of service temperatures behind the 35min, are closed ultra-sonic generator under ultrasonication, and the material that obtains enters next step;
(3) neutralization precipitation: in stirring the neutralization precipitation still, under agitation condition, adding neutralizing agent MgO adjusting pH value is 3-5, makes insoluble impurities separate out removal of impurities;
(4) solid-liquid separation and purification: in the vacuum filtration solid-liquid separating equipment, the previous step material is filtered, filtrate is used mishmetal concentration in the EDTA complexometric titration leach liquor, and obtaining the rare earth leaching rate is 96%, and the liquid phase filtrate that obtains further goes separation and purification to obtain rare-earth products again; Solid phase solid-liquid after washing separates, and the solid phase Separation and Recovery has valence component, and liquid phase is recyclable.
Remove the various embodiments described above, used equipment also can be selected the supersonic leaching equipment of other mentioned in technical solution of the present invention structural shape for use, all can satisfy requirement of the present invention, selects for use different equipment little to leaching isolating influence; The ultrasonic frequency of ultrasonic generator, ultrasonication intensity have considerable influence to leaching isolating speed and efficient.Embodiment of the present invention are a lot, can't be exhaustive, as long as, all belong to protection scope of the present invention in rare earth leaching process all technical schemes with use supersonic leaching equipment.
Claims (5)
1, a kind of method of hypersonic rare earth leaching, with the using rear earth ore sulfuric acid calcination products is raw material, with water is leaching agent, the separation and purification rare earth, it is refining that its step includes batching, leaching, neutralization precipitation, solid-liquid separation, it is characterized in that: described leaching is a supersonic leaching, and supersonic leaching is to carry out in having the supersonic leaching equipment of ultrasonic generator, and its ultrasonication intensity is 0.2～20.0W/cm
2, ultrasonic frequency is 19～80kHz.
2, the method for hypersonic rare earth leaching according to claim 1 is characterized in that: described ultrasonication intensity is 2.0～5.0W/cm
2, ultrasonic frequency is 19～25kHz.
3, the method for hypersonic rare earth leaching according to claim 1 is characterized in that: the solid-to-liquid ratio of leaching using rear earth ore sulfuric acid calcination products and water is 1g: 5ml to 1g: 30ml, and service temperature is 5～60 ℃.
4, the method for hypersonic rare earth leaching according to claim 3 is characterized in that: the service temperature of described leaching is 25～40 ℃.
5, the method for hypersonic rare earth leaching according to claim 1, it is characterized in that: described supersonic leaching equipment comprises leaching container and ultrasonic generator, described leaching container is still formula or slot type or tube container, and described ultrasonic generator is any in probe type ultrasonic wave producer, vibrator type ultrasonic generator, the vibration plate formula ultrasonic generator.
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| CNB2007100199443A CN100424200C (en) | 2007-02-05 | 2007-02-05 | Method for hypersonic rare earth leaching |
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| CNB2007100199443A CN100424200C (en) | 2007-02-05 | 2007-02-05 | Method for hypersonic rare earth leaching |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010081193A1 (en) * | 2009-01-13 | 2010-07-22 | Cavitus Pty Ltd | Mass transfer |
| CN102220493A (en) * | 2011-07-27 | 2011-10-19 | 昆明冶金研究院 | Method and device for purifying zinc sulfate solution based on action of cavitation effect |
| CN103924073A (en) * | 2014-04-28 | 2014-07-16 | 包头稀土研究院 | Method for decomposing rare earth ore concentrate through roasting by liquid caustic soda and acid-leaching rare earth through intensifying by ultrasonic |
| CN105463190A (en) * | 2015-12-31 | 2016-04-06 | 包头稀土研究院 | Method for ultrasonic leaching of acid-process rare earth roasted ore |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| SU1144727A1 (en) * | 1983-09-16 | 1985-03-15 | Бронницкая геолого-геохимическая экспедиция | Method of extracting cryolite from rare-metal raw material |
| CN100348748C (en) * | 2004-12-15 | 2007-11-14 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
-
2007
- 2007-02-05 CN CNB2007100199443A patent/CN100424200C/en not_active Expired - Fee Related
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2010081193A1 (en) * | 2009-01-13 | 2010-07-22 | Cavitus Pty Ltd | Mass transfer |
| CN102220493A (en) * | 2011-07-27 | 2011-10-19 | 昆明冶金研究院 | Method and device for purifying zinc sulfate solution based on action of cavitation effect |
| CN102220493B (en) * | 2011-07-27 | 2013-06-19 | 昆明冶金研究院 | Method and device for purifying zinc sulfate solution based on action of cavitation effect |
| CN103924073A (en) * | 2014-04-28 | 2014-07-16 | 包头稀土研究院 | Method for decomposing rare earth ore concentrate through roasting by liquid caustic soda and acid-leaching rare earth through intensifying by ultrasonic |
| CN105463190A (en) * | 2015-12-31 | 2016-04-06 | 包头稀土研究院 | Method for ultrasonic leaching of acid-process rare earth roasted ore |
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| CN100424200C (en) | 2008-10-08 |
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Granted publication date: 20081008 Termination date: 20120205 |