CN111484064A - Method for recovering cerium and fluorine from bastnaesite leaching solution - Google Patents
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- C—CHEMISTRY; METALLURGY
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Abstract
A process for recovering cerium and fluorine from the leached liquid of bastnaesite includes such steps as adding 0.02-10 g/L g of boric acid to the leached liquid of sulfuric acid, extracting cerium from the liquid by extractant, back extracting, depositing, separating and calcining to obtain CeO2(ii) a Then taking trialkyl phosphine oxide as F in the extraction raffinate, and performing back extraction by using KOH solution to obtain KBF4. The cerium and fluorine proposed by the method are separately recovered, and F is prepared into KBF in the stripping solution4The problems that the mixing clarifying tank is easily blocked and organic phase loss is caused by the organic phase carried by the cerium fluoride precipitate in the operation process of the extraction working section are avoided. The invention uses the extracting agents P507 and P204 to recover Ce, thereby reducing Cyanex923, and the cost is reduced. Comparative CeF of the invention3For products, KBF4The product has more definite market demand and higher added value, and the method is more in line with the market demand and the enterprise demand.
Description
Technical Field
The invention relates to a recovery method, in particular to a method for recovering cerium and fluorine from bastnaesite leachate.
Background
The rare earth resources of Baotou in China are mainly mixed ores of bastnaesite and monazite, and the relative content of the bastnaesite and the monazite is 9:1-1: 1. Wherein the bastnaesite is a cerium fluorocarbon mineral, and the theoretical chemical components are as follows: REO 74.77%, CO220.17 percent of cerium and 8.73 percent of F, and rare earth oxide mainly contains cerium group rare earth elements, so that bastnaesite is an important mineral for extracting cerium and lanthanum, many researches in the prior art are carried out to extract and separate cerium and other rare earth elements from baotite rare earth concentrate, the method comprises the steps of oxidizing trivalent cerium in a cerium-containing mineral or other cerium-containing mixtures into tetravalent cerium, adding acid liquor for leaching, extracting tetravalent cerium in acid leaching liquor, and thus realizing separation of cerium and other rare earth elements, researchers also realize recovery of associated resources F and P in rare earth ore while recovering cerium, and further realizing a clean recovery process, for example, Chinese patent No. 201510571527.4 discloses a method for extracting and separating cerium, fluorine and phosphorus from sulfuric acid leaching liquor of rare earth ore, and the method comprises the following steps of (1) using rare earth sulfate solution obtained by oxidizing and roasting baotite-sulfuric acid leaching or using rare earth sulfate solution obtained by alkali decomposition of rare earth ore solution-wet air oxidation-sulfuric acid leaching as raw material solution, wherein the raw material solution contains L g/50 g of 10-50 g of baotite2，CeO 220 to 80 percent of/REO, 0.5 to 10 g/L of F, 0.5 to 5 g/L of P, and (2) adjusting the acidity of the raw material liquid to 1.5 to 3 mol/L H2SO4Extracting the feed liquid obtained in the step (2) by using an extraction liquid at room temperature, wherein the washing liquid is sulfuric acid with the concentration of 0.5-3 mol/L, the flow ratio of an organic phase of the extraction liquid, the feed liquid and the washing liquid is 1-4: 1: 0.2-1, the stage number of an extraction section is 2-15, the stage number of a washing section is 1-10, the balance time is 1-15 min, and a loaded organic phase containing cerium (IV), fluorine and phosphorus and raffinate are obtained after extraction;(4) at room temperature, the load organic phase containing cerium (IV), fluorine and phosphorus is back-extracted by back extraction liquid to obtain the carrier organic phase containing Ce3+、CeF3And CePO4The back extraction mixture is filtered to obtain the CeF3And CePO4Mixed fine powder and Ce3+A solution; obtained Ce3+Adjusting the pH of the solution to 1-2 by ammonia water, adding oxalic acid to precipitate cerium (III), washing the precipitate, and roasting at 800 ℃ to obtain a product CeO2(ii) a The stripping solution is hydrogen peroxide solution, wherein the volume percentage concentration of the hydrogen peroxide is 0.1-10%; the volume ratio of the stripping solution to a loaded organic phase containing cerium (IV), fluorine and phosphorus is 0.5-2: 1. The method separates cerium, fluorine and phosphorus by a solvent extraction method under proper process conditions, and simultaneously realizes the recovery of F and P in Baotou rare earth ore; the process flow is simple, the yield is high, and the associated F, P resource is recovered, so the method is a clean process method. In the process, the recovery rate of cerium (IV) is more than 95%, the extraction recovery rate of F is more than 93%, the extraction recovery rate of P is more than 95%, and CeO is obtained2Product and CeF3And CePO4Mixing CeO in the micropowder299-99.9999% of REO, ThO2/TCeO<0.01 percent. However, the main problems of the process are as follows: (1) cerium fluoride precipitates are easy to cause blockage of a mixer-settler in the operation process of an extraction working section, and in addition, the problem of organic phase loss caused by the fact that organic phases are carried by the cerium fluoride precipitates is also obvious; (2) the extractant Cyanex923 used in the cerium-fluorine co-recovery process is an imported extractant, so that the cost is high, and the consumption of the Cyanex923 is large due to the high cerium content, so that the process cost is high.
Disclosure of Invention
The invention aims to solve the technical problems in the prior art and provides a method for recovering cerium and fluorine from bastnaesite leachate, which provides that cerium and fluorine are separately recovered, the recovery of Ce is replaced by cheaper commercial extractants P507 and P204, a small amount of F is recovered and used for C923, so that the using amount of Cyanex923 is greatly reduced, and the cost is reduced; the method prepares F into KBF in the back extraction solution4The obtained product has more definite market demand.
In order to solve the technical problems, the technical scheme of the invention is as follows:
the invention provides a method for recovering cerium and fluorine from bastnaesite leaching solution, which comprises the following steps:
takes the sulfuric acid leaching solution of bastnaesite or the mixed ore of bastnaesite and monazite as raw material solution, and the composition of the raw material solution is 10-60 g/L CeO2，CeO2The REO accounts for 20-80 wt%, the total content of rare earth oxide, 1-12 g/L F, and the acidity of the feed liquid is 1.5-2.5 mol/L H2SO4(ii) a The diluent is a mixture of two or more alkanes or aromatics in hydrocarbons containing 6-20C atoms;
(1) adding 0.02-10 g/L of boric acid into the feed liquid;
(2) the extracting agent is H L (monobasic phosphate P204 (di (2-ethylhexyl) phosphate) or phosphonic acid P507 (2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester)), and the extracting agent is diluted by a diluent and is used for extracting the feed liquid in the step (1) to obtain a cerium-containing organic phase and raffinate containing F and other trivalent rare earths;
(3) the cerium-containing organic phase is subjected to back extraction, precipitation, separation and roasting by using a back extraction solution to obtain CeO2；
(4) Taking trialkyl phosphine oxide (Cyanex923) as an extracting agent, and using an extraction liquid obtained after dilution with a diluent to extract raffinate containing F and other trivalent rare earths to obtain an organic phase containing B-F and an extraction liquid of other trivalent rare earths; then the organic phase containing B-F is subjected to back extraction by KOH solution, and the pH value of the B-F back extraction solution is adjusted after the back extraction is finished until KBF is separated out4Solid, centrifugally separated, washed and dried to obtain KBF4。
In the technical scheme, in the step (2), the flow ratio of the organic phase to the feed liquid to the washing liquid is preferably 1-4: 1: 0.5-1, and the washing liquid is preferably 0.1-2 mol/L of H2SO4The number of extraction stages is 4-10 stages, and the number of washing stages is 1-5 stages.
In the above technical solution, preferably, the step (3) specifically includes the following steps:
the cerium-containing organic phase is subjected to back extraction by using a back extraction solution, wherein the back extraction solution comprises 0.5-5% of hydrogen peroxide and 0-3 mol/L of sulfuric acid or nitreAcid, ammonia water is used for adjusting the pH value to 1.8-2, oxalic acid is added for precipitation, and CeO is obtained by precipitation, separation, washing and roasting2The recovery rate of Ce is more than 90 percent, and the purity of CeO2The ratio of/REO is 99-99.99%.
In the above technical solution, it is preferable that the volume fraction of the trialkyl phosphine oxide (Cyanex923) in the extract liquid in the step (4) is 0.5 to 10%.
In the above technical solution, it is preferable that the extraction step in the step (4) is performed by extraction separation according to the ratio of O: a ═ 1.
In the above technical solution, preferably, the mass fraction of the KOH solution in the step (4) is 1-5%.
In the above technical solution, preferably, after the back extraction in step (4) is completed, the pH of the B-F back extraction solution is adjusted to 3-4.4 with ammonia water until KBF is precipitated4And (3) a solid.
In the above-mentioned aspect, it is preferable that the KBF obtained in the step (4)4Wherein the yield of F is greater than 95%, the KBF obtained4The mass fraction of solids is more than or equal to 97 percent.
The invention has the beneficial effects that:
compared with the process for preparing cerium fluoride by cerium-fluorine co-extraction, the method has the advantages that:
1. the cerium and fluorine proposed by the method are separately recovered, and F is prepared into KBF in the stripping solution4The problems that the mixing clarifying tank is easily blocked and organic phase loss is caused by the organic phase carried by the cerium fluoride precipitate in the operation process of the extraction working section are avoided.
2. The method of the invention replaces the recycle of Ce with cheaper commercial extracting agents P507 and P204, recycles a small amount of F to use C923, greatly reduces the dosage of Cyanex923 and reduces the cost.
3. Method of the invention comparison with CeF3For products, KBF4The product has more definite market demand and higher added value, and the method is more in line with the market demand and the enterprise demand.
Drawings
The present invention will be described in further detail with reference to the accompanying drawings and specific embodiments.
FIG. 1 shows KBF obtained in example 1 of the present invention4XRD pattern of (a).
Detailed Description
Example 1
A process for recovering cerium and fluorine from sulfuric acid leaching solution of bastnaesite as raw material liquid containing 30 g/L g of CeO2，CeO 240 percent of REO, the total content of the rare earth oxides of the REO, 6 g/L of F feed liquid, the acidity of the F feed liquid is 2.0 mol/L H2SO4. The diluent is n-heptane and n-octane, and the volume ratio of the two is 1: 1.
(1) Adding 5 g/L of boric acid into the feed liquid;
(2) the extracting agent is H L (monobasic phosphate P204 (di (2-ethylhexyl) phosphoric acid), the volume fraction of the extracting agent is 10% by diluting with a diluent, the extracting agent is used for extracting the feed liquid in the step (1), the flow ratio of the organic phase to the feed liquid to the washing liquid is 2.5: 1:0.75, and the washing liquid is 1 mol/L of H2SO4. The extraction stage number is 7, the washing stage number is 3, and a cerium-containing organic phase and raffinate containing F and other trivalent rare earths are obtained;
(3) the composition of back extraction solution for cerium-containing organic phase is 2.5% of hydrogen peroxide and 2 mol/L of sulfuric acid, the pH value is adjusted to 1.8 by ammonia water, oxalic acid is added for precipitation, and the precipitate is separated, washed and roasted to obtain CeO2The recovery rate of Ce is more than 90 percent, and the purity of CeO2The ratio of/REO is 99-99.99%.
(4) F in the raffinate is extracted and separated by taking trialkyl phosphine oxide (Cyanex923) as an extracting agent and diluting the trialkyl phosphine oxide with n-heptane to 5 volume percent according to the proportion of O to A being 1. Obtaining the organic phase containing B-F and the extraction liquid of other trivalent rare earths. Then, the B-F loaded organic phase is subjected to back extraction by using a KOH solution with the mass fraction of 3%, after the back extraction is finished, the pH of the B-F back extraction solution is adjusted to 3 by using ammonia water, and KBF is separated out4Solid, centrifugally separated, washed and dried to obtain KBF4. Wherein the yield of F is more than 95%, and the obtained KBF4The mass fraction of solids is more than or equal to 97 percent.
FIG. 1 shows the KBF obtained4The XRD pattern of (A) shows that: this example gives KBF4So that fluorine carbon ceriumKBF of F recovered from sulfuric acid leaching solution of ore4Exist in the form of (1).
Example 2
The process for recovering cerium and fluorine from sulfuric acid leaching solution of bastnaesite and monazite mixed ore comprises 10 g/L g of CeO as raw material liquid2，CeO2The weight percentage of REO is 20 percent, the REO is the total content of rare earth oxides, 1 g/L F feed liquid acidity is 1.5 mol/L H2SO4. The diluent is n-heptane and n-octane, and the volume ratio of the two is 1: 1.
(1) Adding 1 g/L of boric acid into the feed liquid;
(2) the extractant is H L phosphonic acid P507 (2-ethylhexyl phosphonic acid mono-2-ethylhexyl ester)), the volume fraction of the extractant is diluted by a diluent to be 5%, the flow ratio of the organic phase to the feed liquid to the washing liquid is 1: 1:0.5, and the washing liquid is 0.1 mol/L of H2SO4. The extraction stage number is 4, the washing stage number is 1, and a cerium-containing organic phase and raffinate containing F and other trivalent rare earths are obtained;
(3) the composition of back extraction solution for cerium-containing organic phase is 0.5% of hydrogen peroxide and 0.5 mol/L nitric acid, ammonia water is used for regulating pH value to 1.8, oxalic acid is added for precipitation, and CeO is obtained by precipitation, separation, washing and roasting2The recovery rate of Ce is more than 90 percent, and the purity of CeO2The ratio of/REO is 99-99.99%.
(4) F in the raffinate is extracted and separated by taking trialkyl phosphine oxide (Cyanex923) as an extracting agent and diluting the trialkyl phosphine oxide with a diluent to 0.5 volume percent according to the proportion of O to A being 1. Obtaining the organic phase containing B-F and the extraction liquid of other trivalent rare earths. Then the organic phase loaded with the B-F is subjected to back extraction by using a KOH solution with the mass fraction of 1%, after the back extraction is finished, the pH of the B-F back extraction solution is adjusted to 3 by using ammonia water, and KBF is separated out4Solid, centrifugally separated, washed and dried to obtain KBF4. Wherein the yield of F is more than 95%, and the obtained KBF4The mass fraction of solids is more than or equal to 97 percent.
Example 3
The cerium and fluorine recovering process with sulfuric acid leaching solution of bastnaesite includes 60 g/L g CeO as material liquid2，CeO280% by weight of REO, the total content of rare earth oxides being REO, and 12 g/LF. The acidity of the feed liquid is 2.5 mol/L H2SO4. The diluent is n-heptane and n-octane, and the volume ratio of the two is 1: 1.
(1) Adding 10 g/L of boric acid into the feed liquid;
(2) the extractant is H L (monobasic phosphate P204 (di (2-ethylhexyl) phosphate), the volume fraction of the extractant is 15% by diluting with a diluent, the flow ratio of the organic phase to the feed liquid to the washing liquid is 4:1: 1, and the washing liquid is 2 mol/L of H2SO4. The extraction stage number is 10 stages, the washing stage number is 5 stages, and a cerium-containing organic phase and raffinate containing F and other trivalent rare earths are obtained
(3) The composition of back extraction solution for cerium-containing organic phase is 5% of hydrogen peroxide and 3 mol/L sulfuric acid, the pH value is adjusted to 2 by ammonia water, oxalic acid is added for precipitation, the precipitate is separated, washed and roasted to obtain CeO2The recovery rate of Ce is more than 90 percent, and the purity of CeO2The ratio of/REO is 99-99.99%.
(4) F in the extract is extracted and separated by taking trialkyl phosphine oxide (Cyanex923) as an extracting agent and diluting the trialkyl phosphine oxide with a diluent until the volume fraction of the extracting agent is 10 percent according to the proportion of O to A being 1. Obtaining the organic phase containing B-F and the extraction liquid of other trivalent rare earths. Then, the B-F loaded organic phase is subjected to back extraction by using a KOH solution with the mass fraction of 5%, after the back extraction is finished, the pH of the B-F back extraction solution is adjusted to 4.4 by using ammonia water, and KBF is separated out4Solid, centrifugally separated, washed and dried to obtain KBF4. Wherein the yield of F is more than 95%, and the obtained KBF4The mass fraction of solids is more than or equal to 97 percent.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (8)
1. A method for recovering cerium and fluorine from bastnaesite leachate is characterized by comprising the following steps:
takes the sulfuric acid leaching solution of bastnaesite or the mixed ore of bastnaesite and monazite as raw material solution, and the composition of the raw material solution is 10-60 g/L CeO2，CeO2The REO accounts for 20-80 wt%, the total content of rare earth oxide, 1-12 g/L F, and the acidity of the feed liquid is 1.5-2.5 mol/L H2SO4(ii) a The diluent is a mixture of two or more alkanes or aromatics in hydrocarbons containing 6-20C atoms;
(1) adding 0.02-10 g/L of boric acid into the feed liquid;
(2) the extracting agent is di (2-ethylhexyl) phosphoric acid or 2-ethylhexyl phosphonic acid mono 2-ethylhexyl ester, and is diluted by a diluent and used for extracting the feed liquid in the step (1) to obtain a cerium-containing organic phase and raffinate containing F and other trivalent rare earths;
(3) the cerium-containing organic phase is subjected to back extraction, precipitation, separation and roasting by using a back extraction solution to obtain CeO2；
(4) Taking trialkyl phosphine oxide as an extracting agent, and using an extraction liquid obtained after dilution by a diluent to extract raffinate containing F and other trivalent rare earths to obtain an organic phase containing B-F and an extraction liquid of other trivalent rare earths; then the organic phase containing B-F is subjected to back extraction by KOH solution, and the pH value of the B-F back extraction solution is adjusted after the back extraction is finished until KBF is separated out4Solid, centrifugally separated, washed and dried to obtain KBF4。
2. The method according to claim 1, wherein in the step (2), the flow ratio of the organic phase to the feed liquid to the washing liquid is 1-4: 1: 0.5-1, and the washing liquid is 0.1-2 mol/L of H2SO4The number of extraction stages is 4-10 stages, and the number of washing stages is 1-5 stages.
3. The method according to claim 1, characterized in that step (3) comprises in particular the steps of:
the cerium-containing organic phase is subjected to back extraction by using a back extraction solution, wherein the back extraction solution comprises 0.5-5% of hydrogen peroxide and 0-3 mol/L of sulfuric acid or nitric acid, the pH value is adjusted to 1.8-2 by using ammonia water, oxalic acid is added for precipitation, and the precipitate is separated, washed and roasted to obtain CeO2The recovery rate of Ce is more than 90 percent, and the purity is highCeO2The ratio of/REO is 99-99.99%.
4. The method of claim 1, wherein the volume fraction of trialkylphosphine oxide in the extract in step (4) is 0.5-10%.
5. The method of claim 1, wherein the extraction step in step (4) is performed according to the comparison of O: a ═ 1.
6. The method according to claim 1, wherein the mass fraction of the KOH solution in the step (4) is 1-5%.
7. The method of claim 1, wherein after the back extraction in step (4), the pH of the B-F back extraction solution is adjusted to 3-4.4 with ammonia water until KBF is precipitated4And (3) a solid.
8. The process according to claim 1, wherein the KBF obtained in step (4)4Wherein the yield of F is greater than 95%, the KBF obtained4The mass fraction of solids is more than or equal to 97 percent.
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| CN110484756A (en) * | 2019-09-24 | 2019-11-22 | 江西沪昌电缆有限公司 | A kind of preparation method of aluminium base high conductivity electric wire |
| CN113800564A (en) * | 2021-08-27 | 2021-12-17 | 稀美资源(广东)有限公司 | Preparation method of niobium oxide and tantalum oxide |
| CN115259204A (en) * | 2022-07-28 | 2022-11-01 | 中国科学院长春应用化学研究所 | Clean metallurgical process method for synchronously recycling cerium and fluorine to treat bastnaesite |
| WO2024124712A1 (en) * | 2022-12-12 | 2024-06-20 | 广东邦普循环科技有限公司 | Method for recovering manganese and fluorine from manganese salt solution |
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| CN113800564A (en) * | 2021-08-27 | 2021-12-17 | 稀美资源(广东)有限公司 | Preparation method of niobium oxide and tantalum oxide |
| CN115259204A (en) * | 2022-07-28 | 2022-11-01 | 中国科学院长春应用化学研究所 | Clean metallurgical process method for synchronously recycling cerium and fluorine to treat bastnaesite |
| CN115259204B (en) * | 2022-07-28 | 2023-08-04 | 中国科学院长春应用化学研究所 | Clean metallurgical process method for synchronously recycling cerium fluoride to treat bastnaesite |
| WO2024124712A1 (en) * | 2022-12-12 | 2024-06-20 | 广东邦普循环科技有限公司 | Method for recovering manganese and fluorine from manganese salt solution |
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