CN102899486B - Method for leaching bastnaesite-containing rare-earth ore concentrates in complexing mode and preparing kryocide - Google Patents
Method for leaching bastnaesite-containing rare-earth ore concentrates in complexing mode and preparing kryocide Download PDFInfo
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- CN102899486B CN102899486B CN201210434070.9A CN201210434070A CN102899486B CN 102899486 B CN102899486 B CN 102899486B CN 201210434070 A CN201210434070 A CN 201210434070A CN 102899486 B CN102899486 B CN 102899486B
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Abstract
The invention discloses a method for leaching bastnaesite-containing rare-earth ore concentrates in a complexing mode and preparing kryocide, and belongs to the technical field of rare-earth hydrometallurgy. The method comprises the following steps of: adding hydrochloric acid with a certain concentration and easily-dissolved fluorides into the bastnaesite-containing rare-earth ore concentrates to remove calcium and iron from the rare-earth ore concentrates, filtering, washing, and adding the hydrochloric acid and aluminum chloride to perform complexing leaching; discomposing bastnaesite in the rare-earth ore concentrates into a solution, so that fluorine and aluminum exist in the solution in a complex mode; and separating rare earth by using a double salt precipitation method, adding kryocide seed crystals into a filtrate, and regulating the pH value of the solution by using alkali liquor to prepare the white kryocide product. The method is operated at low temperature in a wet method, and is low in cost, small in pollution to environment and high in economic benefits, energy consumption is reduced greatly, and equipment is simple.
Description
technical field
The present invention relates to a kind of rare earth ore concentrate containing hamartite and prepare the method for sodium aluminum fluoride, belong to rare-earth wet method metallurgical technology field.
background technology
The mixed type rare-earth mineral that comprises the mineral such as single hamartite and hamartite and monazite containing the rare earth ore concentrate of hamartite.Hamartite chemical formula can be expressed as REFCO
3or REF
3rE
2(CO
3)
3, be the complex chemical compound of rare earth carbonate and rare earth fluorine.This mineral be mainly distributed in the U.S. California, the Bayan Obo in China Inner Mongol, the ground such as Weishan County in the Mianning County in Sichuan, Shandong.Hamartite decomposes is rare earth oxide and oxyfluoride, then by acidleach, alkali, soaks or the soda acid method Extraction of rare earths such as leaching that go forward one by one.
At present, for single type hamartite with containing the various decomposition methods of the mixed type rare-earth mineral of hamartite, being summed up is exactly mainly acid system and alkaline process, and acid system mainly adopts hydrochloric acid or sulfuric acid, in concentrated sulfuric acid roasting method, existence due to fluorine element, make in this technological process easily to produce HF gas and sulfuric acid mist, contaminate environment but also large to equipment corrosion not only, technical process is long, raw material consumption amount is large, and this method is eliminated gradually.First hydrochloric acid rule need to be decomposed into rare earth oxide by mineral high-temperature roasting, emit HF gas simultaneously, this method can obtain the mishmetal feed liquid of higher concentration, and facility investment is few, technique is simple, applies comparatively extensively, and for example Chinese patent CN 101967555 A disclose a kind of method that leaches again Bastnaesite after activation, carry out according to the following steps: (1) at 100 ~ 400 ℃ of roasting 1 ~ 4h, makes activation ore deposit by hamartite; (2) will activate mining hydrochloric acid soln and leach under agitation condition, then filtering separation leach liquor; (3) under agitation condition, in leach liquor, add rare earth hydrate, then filter and obtain first-time filtrate; (4) by first-time filtrate extraction, obtain extraction phase and extracting phase; (5) extraction phase is stripped with hydrochloric acid soln, obtaining water is the solution that contains rare earth chloride.
Alkaline process is to adopt dense NaOH decomposition method and carbonate decomposition method, and NaOH decomposition method is to adopt dense NaOH to decompose mineral.Carbonate decomposition method adopts alkaline carbonate conventionally, as a kind of disclosed method in the publication number Chinese patent that is CN1205363A be with alkaline carbonate and hamartite baking mixed after, washing defluorination, then the sour molten rare earth chloride liquid that obtains, extracting and separating can obtain single rare earth product, and the method can alleviate the pollution of fluorine to environment.But alkaline process is high to mineral grade requirement, equipment erosion resistance is required strictly, alkaline consumption is large, and produces waste water containing fluorine, if do not processed, same contaminate environment.
The root problem that above method exists is all cannot solve the problem of the recycling of fluorine element in Baotou rare earth ore deposit, fluorine is entered in atmosphere or waste water, contaminate environment.
In Baotou rare earth ore concentrate, the content of fluorine is about 3～8%, therefore fluorine is reclaimed and is converted into available product and be significant.
Summary of the invention
The technical issues that need to address of the present invention are just to overcome the defect of prior art, a kind of rare earth ore concentrate complexation leaching and sodium aluminum fluoride preparation method containing hamartite is provided, it decomposes mixed rare earth concentrates fully by chemical decomposition method, and fluorine element is converted into sodium aluminum fluoride, fluorine element is reclaimed fully, and energy consumption is little, and environmental pollution is little, concentrate rate of decomposition is high, and economic benefit is high.
For addressing the above problem, the present invention adopts following technical scheme:
The invention provides a kind of rare earth ore concentrate complexation leaching and sodium aluminum fluoride preparation method containing hamartite, operation steps is as follows:
(1) deliming and iron: the rare earth ore concentrate containing hamartite adds after fluorochemical and hydrochloric acid, removes calcium and iron in concentrate, filter also and obtain filtrate I and filter residue I after washing leaching cake;
(2) complexation leaching: add HCl solution and AlCl in filter residue I
3solid, filters after complexation leaching, obtains filtrate II;
(3) double salt precipitation: add vitriol to carry out double salt precipitation in filtrate II, obtain filtrate III and double salt of rare earth throw out thing after filtration;
(4) adjust pH: add sodium aluminum fluoride crystal seed post-heating to stir in filtrate III, and regulate the pH value of filtrate between 3.5-4.5 with basic solution, three the washing post-dryings of solid that obtain after solid-liquid separation, obtain white ice spar product.
Rare earth ore concentrate containing hamartite is Mianning hamartite or the U.S. awns Yan Pasikuang in packet header mixed rare earth concentrates, Sichuan, hamartite content >=30%.
The condition of the hydrochloric acid deliming described in step (1) and iron is: in the Sealing Arrangement with condenser system, concentration of hydrochloric acid 3mol/L, liquid-solid ratio is 8:1,95 ℃ of temperature, at the uniform velocity stir 2 hours, fluorochemical add-on is 2～5% of hamartite middle rare earth weight content, and fluorochemical is to be soluble in sour fluorochemical hydrofluoric acid HF, fluorite CaF
2, aluminum fluoride AlF
3, Sodium Fluoride NaF or Potassium monofluoride KF, after reaction finishes, be cooled to 55 ℃ of filtrations.
Complexation leaching condition described in step (2) is: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, filter after simultaneously at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times.
In step (3), double salt precipitation vitriol used is K
2sO
4, Na
2sO
4in a kind of or two kinds, the temperature of double salt precipitation is 95 ℃, vitriol and solution middle rare earth, in mass ratio for 4:1 adds, filter after uniform stirring 60min, obtain filtrate III and double salt of rare earth throw out.
Described in step (4), filtrate III is heated to 55 ℃, by concentration, is less than NaOH, the KOH of 0.1mol/L or ammoniacal liquor, the NH that is 1.5mol/L by concentration
4hCO
3, NaHCO
3, Na
2cO
3in at least one regulator solution pH be 3.5-4.5, continue to stir after 60min and filter, washing, dry and obtain the white ice spar that contains trace rare-earth, this sodium aluminum fluoride is Na
3alF
6or K
3alF
6or Na
3alF
6and K
3alF
6mixture.
The filtrate I obtaining in step (1) recycles.
Step (4) obtains, containing Al filtrate, recycling.
In step of the present invention (1), adding the object that is soluble in sour fluorochemical is that rare earth and fluorine have very strong bonding force in order to prevent that fluorine carbonated rare earth can be partly dissolved in hydrochloric acid in the loss of deironing calcium process middle-weight rare earths, easily form rare earth fluoride precipitation, thereby stayed, soak in slag.
In step (2), after Leaching in Hydrochloric Acid, the object of heat filtering is, after preventing that Cucumber from reducing with temperature, because solubleness reduces, to separate out.
In step (3), because of the rising of the solubility with temperature of rare earth sulfuric acid sodium double salt or rare earth sulfuric acid potassium double salt, reduce, so double salt precipitation temperature is selected 95 ℃ of the bests.
In step (4), during the pH of regulator solution, if use highly basic to regulate, concentration of lye must be less than 0.1mol/L so, if use weak base to regulate, concentration of lye is that 1.5 mol/L are best so, because if concentration of lye is too high, after adding while regulating pH value, can produce immediately rare earth hydrate precipitation, if the too fast rare earth hydrate precipitation that also can produce adding.
Thereby advantage of the present invention has:
Decomposition method with respect to hamartite in the past, the present invention has saved the process of oxidizing roasting, adopted hydrometallurgical technology, according to fluorine aluminium complex scheme, promoted the decomposition of mixed rare earth concentrates, and prevented overflowing of fluorine element, be effectively translated into sodium aluminum fluoride, in this sodium aluminum fluoride, contained a small amount of rare earth element, can directly apply in Aluminum Electrolysis Production, reduce rare earth and added step, be conducive to the quality of aluminium product, cost-saving, reduce operation, technique is simple, easily controls, and has good economic benefit and environmental benefit.This kind of method for decomposing hamartite is simple, and cost is low, low for equipment requirements, is easy to realize suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is of the present invention containing the rare earth ore concentrate complexation leaching of hamartite and sodium aluminum fluoride preparation method's schema.
Embodiment
embodiment 1
As shown in Figure 1, take Mianning, sichuan Province hamartite 2kg, rare earth oxide content is 61.5%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 5ml analytical pure hydrofluoric acid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By K
2sO
4, in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min with solution middle rare earth, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, slowly adds alkali lye after adding sodium aluminum fluoride crystal seed, and the NaOH that is 0.08mol/L by concentration regulates pH to 3.5 left and right, continues to stir after 60min and filters, washing, dries and obtain white potassium cryolite K
3alF
6, in this sodium aluminum fluoride, containing rare earth oxide, be 0.13%.
Obtain containing Al filtrate, recycle.
embodiment 2
As shown in Figure 1, take Mianning, sichuan Province hamartite 2kg, rare earth oxide content is 61.5%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 7g Sodium Fluoride solid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By K
2sO
4, in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min with solution middle rare earth, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, adds after sodium aluminum fluoride crystal seed the pH to 3.7 of the ammoniacal liquor regulator solution that is 1.5mol/L by concentration, continues to stir after 60min and filters, washing, dries and obtain white potassium cryolite K
3alF
6, in this sodium aluminum fluoride, containing rare earth oxide, be 0.21%.
Obtain containing Al filtrate, recycle.
embodiment 3
As shown in Figure 1, take packet header mixed rare earth concentrates 2kg, hamartite content is 41.06%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 6g Calcium Fluoride (Fluorspan) solid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By Na
2sO
4, in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min with solution middle rare earth, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, adds after sodium aluminum fluoride crystal seed the NH that is 1.5mol/L by concentration
4hCO
3the pH to 3.8 of regulator solution, filtration after continuation stirring 60min, washing, oven dry obtain white sodium cryolite Na
3alF
6, in this sodium aluminum fluoride, containing rare earth oxide, be 0.37%.
Obtain containing Al filtrate, recycle.
embodiment 4
As shown in Figure 1, take U.S. awns and prolong Paasche rare earth ore concentrate 2kg, hamartite content is 38.52%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 5g aluminum fluoride solid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By Na
2sO
4, in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min with solution middle rare earth, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, adds after sodium aluminum fluoride crystal seed the Na that is 1.5mol/L by concentration
2cO
3the pH to 4.0 of regulator solution, filtration after continuation stirring 60min, washing, oven dry obtain white sodium cryolite Na
3alF
6, in this sodium aluminum fluoride, containing rare earth oxide, be 0.24%.
Obtain containing Al filtrate, recycle.
embodiment 5
As shown in Figure 1, take packet header mixed rare earth concentrates 2kg, hamartite content is 65.12%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 8g Sodium Fluoride solid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By Na
2sO
4and K
2sO
4mixture and solution middle rare earth in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, adds after sodium aluminum fluoride crystal seed the Na that is 1.5mol/L by concentration
2cO
3the pH to 4.2 of regulator solution, filtration after continuation stirring 60min, washing, oven dry obtain white sodium potassium mixing sodium aluminum fluoride, and in this sodium aluminum fluoride, containing rare earth oxide is 0.69%.
Obtain containing Al filtrate, recycle.
embodiment 6
As shown in Figure 1, take packet header mixed rare earth concentrates 2kg, hamartite content is 65.12%.In the Sealing Arrangement with condenser system, by liquid-solid ratio, be the hydrochloric acid that 8:1 adds 3mol/L, add 9g Potassium monofluoride solid, be heated to after 95 ℃, add above concentrate, at the uniform velocity stir 2 hours, reaction obtains filtrate I and filter residue after being cooled to 55 ℃ to filter and wash after finishing.Filtrate I recycles.
In filter residue, add HCl solution and AlCl
3solid, according to following condition complexation leaching: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, is cooled to 85 ℃ of heat filterings after at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times, obtains filtrate II.
By Na
2sO
4and K
2sO
4mixture and solution middle rare earth in mass ratio for 4:1 adds in filtrate II, at 95 ℃, filter after at the uniform velocity stirring 60min, obtain filtrate III and double salt of rare earth throw out.Filtrate III is heated to 55 ℃, the pH to 4.5 that adds after sodium aluminum fluoride crystal seed the NaOH regulator solution that is 0.06mol/L by concentration, filtration after continuation stirring 60min, washing, oven dry obtain white sodium potassium mixing sodium aluminum fluoride, and in this sodium aluminum fluoride, containing rare earth oxide is 0.69%.
Obtain containing Al filtrate, recycle.
Finally it should be noted that: obviously, above-described embodiment is only for example of the present invention is clearly described, and the not restriction to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without also giving all embodiments.And the apparent variation of being amplified out thus or change are still among protection scope of the present invention.
Claims (4)
1. containing the rare earth ore concentrate of hamartite, prepare a method for sodium aluminum fluoride, it is characterized in that, operation steps is as follows:
(1) deliming and iron: the rare earth ore concentrate containing hamartite adds after fluorochemical and hydrochloric acid, removes calcium and iron in concentrate, filter also and obtain filtrate I and filter residue I after washing leaching cake;
The condition of deliming and iron is: in the Sealing Arrangement with condenser system, concentration of hydrochloric acid 3mol/L, liquid-solid ratio is 8:1,95 ℃ of temperature, at the uniform velocity stir 2 hours, fluorochemical add-on is 2～5% of hamartite middle rare earth weight content, and fluorochemical is to be soluble in sour fluorochemical hydrofluoric acid HF, fluorite CaF
2, aluminum fluoride AlF
3, Sodium Fluoride NaF or Potassium monofluoride KF, after reaction finishes, be cooled to 55 ℃ of filtrations;
(2) complexation leaching: add HCl solution and AlCl in filter residue I
3solid, filters after complexation leaching, obtains filtrate II;
Complexation leaching condition is: in the Sealing Arrangement with condenser system, HCl concentration is 6mol/L, AlCl
3concentration is 2mol/L, and extraction temperature is 110 ℃, and liquid-solid ratio is 30:1, filter after simultaneously at the uniform velocity stirring 90min, and with 85 ℃ of distilled water wash filter residues 3 times;
(3) double salt precipitation: add vitriol to carry out double salt precipitation in filtrate II, obtain filtrate III and double salt of rare earth throw out thing after filtration;
Double salt precipitation vitriol used is K
2sO
4, Na
2sO
4in a kind of or two kinds, the temperature of double salt precipitation is 95 ℃, vitriol and solution middle rare earth, in mass ratio for 4:1 adds, filter after uniform stirring 60min, obtain filtrate III and double salt of rare earth throw out;
(4) adjust pH: add sodium aluminum fluoride crystal seed post-heating to 55 ℃ in filtrate III, be less than NaOH, the KOH of 0.1mol/L or ammoniacal liquor, the NH that is 1.5mol/L by concentration by concentration
4hCO
3, NaHCO
3, Na
2cO
3in at least one regulator solution pH be 3.5-4.5, continue to stir after 60min and filter, washing, dry and obtain the white ice spar that contains trace rare-earth, this sodium aluminum fluoride is Na
3alF
6or K
3alF
6or Na
3alF
6and K
3alF
6mixture.
2. the rare earth ore concentrate containing hamartite as claimed in claim 1 is prepared the method for sodium aluminum fluoride, it is characterized in that, rare earth ore concentrate containing hamartite is Mianning hamartite or the U.S. awns Yan Pasikuang in packet header mixed rare earth concentrates, Sichuan, hamartite content >=30%.
3. the rare earth ore concentrate containing hamartite as claimed in claim 1 or 2 is prepared the method for sodium aluminum fluoride, it is characterized in that, the filtrate I obtaining in step (1) recycles.
4. the rare earth ore concentrate containing hamartite as claimed in claim 3 is prepared the method for sodium aluminum fluoride, it is characterized in that, step (4) obtains, containing Al filtrate, recycling.
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| CN102146512A (en) * | 2010-02-08 | 2011-08-10 | 北京有色金属研究总院 | Hamartite smelting separation process |
| CN102653823A (en) * | 2012-05-25 | 2012-09-05 | 东北大学 | Method used for separating rare earth from bastnaesite sulphuric acid leach solution and preparing ice stone |
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