CN115652113A - Method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution - Google Patents
Method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution Download PDFInfo
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Abstract
The invention discloses a method for extracting and separating rare earth from a marine rare earth sulfuric acid leaching solution, which comprises the following steps: extracting the marine rare earth sulfuric acid leaching solution by adopting a secondary carbon primary amine extractant-tributyl phosphate-sulfonated kerosene mixed extractant to obtain a rare earth-containing load organic phase and a raffinate aqueous phase; carrying out back extraction on the rare earth-containing loaded organic phase obtained in the step 1) by using hydrochloric acid to obtain a separated rare earth back extraction solution; the invention skillfully utilizes the mixed extractant of N1923-TBP-sulfonated kerosene to react with rare earth ions and Fe in a sulfate system and a chloride system 3+ And other non-rare earth impurities to finally realize the selective extraction characteristic difference between rare earth ions and Fe in the marine rare earth sulfuric acid leaching solution 3+ And other non-rare earth impurity ions are completely separated, the separation effect is good, the process is simple, and the recovery rate is high.
Description
The technical field is as follows:
the invention relates to the technical field of hydrometallurgy, in particular to a method for extracting and separating rare earth from a marine rare earth sulfuric acid leaching solution.
Background art:
the rare earth elements have rich and unique magnetic, optical and electric properties and are non-renewable precious mineral resources. In recent years, with the gradual decline of the reserves of the rare earth resources on land, the high-grade rare earth resources which can be developed and utilized are about to be exhausted, and the development of the marine rare earth resources is concerned more and more widely.
The characteristics of the minerals of the marine rare earth have typical differences due to the difference of the mining process of the marine rare earth and the land rare earth. In a slow geological process, rare earth and alkali metals such as Ca, sr, ba and the like compete to combine with phosphate ions in seawater. The rare earth-rich phosphate mineral is formed through chemical precipitation, biomineralization and diagenesis of organic P, so that the phosphate mineral becomes a rare earth element carrier mineral in deep sea sediments. Because of the small solubility product of the rare earth phosphate, the KSP is 10 at 25 DEG C -23 On the other hand, it is soluble only in a strongly acidic system. On the basis of comprehensive consideration of the aspects of cost, safety, equipment requirement and the like, sulfuric acid is the preferred acid leaching agent, and the obtained marine rare earth sulfuric acid leaching solution has high acidity (pH = -0.5-1.5) and Fe 3+ 、Al 3+ The like, high impurity concentration, complete rare earth distribution (containing rare earth elements such as La-Lu, Y, sc and the like) and low concentration, and the like, so that the difficulty in extracting the rare earth is obviously increased. How to realize the high-efficiency extraction and separation of rare earth and non-rare earth impurities in the marine rare earth sulfuric acid leaching solution is a key problem which restricts the development and utilization of marine rare earth resources.
However, the existing extractant system and extraction technology are difficult to be well applied to the sulfuric acid leaching solution system for efficiently extracting and separating the rare earth. In view of this, the invention is particularly proposed.
The invention content is as follows:
the invention aims to provide a method for extracting and separating rare earth from a marine rare earth sulfuric acid leaching solution.
The invention is realized by the following technical scheme:
a method for extracting and separating rare earth from a marine rare earth sulfuric acid leaching solution comprises the following steps:
1) Extracting the marine rare earth sulfuric acid leaching solution by using a secondary carbon primary amine extractant (N1923) -tributyl phosphate (TBP) -sulfonated kerosene mixed extractant to obtain a rare earth-containing load organic phase and a raffinate aqueous phase; wherein, the secondary carbon primary amine extractant (N1923) -tributyl phosphate (TBP) -sulfonated kerosene mixed extractant is prepared from the secondary carbon primary amine extractant (N1923), the tributyl phosphate (TBP) and sulfonated kerosene with the volume ratio of 1-3:1-3:4-8; the rare earth ion contained in the rare earth sulfuric acid leaching liquid is 200-500 mg/L, fe 3+ 0.5～2g/L、Al 3+ 5～10g/L、Mn 2+ 1～5g/L、Mg 2+ 1-10 g/L and Ca 2+ 0.5～1.0g/L；
2) And (2) carrying out back extraction on the rare earth-containing loaded organic phase obtained in the step 1) by using hydrochloric acid to obtain a separated rare earth back extraction solution.
Preferably, the extraction mode of the step 1) is countercurrent or cross-current extraction; the extraction phase ratio O/A is 1; the extraction stage number is 1-3; the extraction time is 5-10 min.
Preferably, hydrochloric acid is adopted to reversely extract the rare earth-containing loaded organic phase in the step 2) in a counter-current or cross-current manner; the back extraction phase ratio O/A is 1-2:1.
Preferably, the hydrochloric acid concentration is 6 to 12mol/L.
Preferably, the stage number of the countercurrent or cross-flow back extraction in the step 2) is 1-3 stages; the back extraction time is 5-10 min.
The pH value of the marine rare earth sulfuric acid leaching solution is = -0.5-1.5.
The invention has the following beneficial effects: the invention skillfully utilizes the mixed extractant of N1923-TBP-sulfonated kerosene to react with rare earth ions and Fe in a sulfate system and a chloride system 3+ And other non-rare earth impurities to finally realize the selective extraction characteristic difference between rare earth ions and Fe in the marine rare earth sulfuric acid leaching solution 3+ And other non-rare earth impurity ionsGood separation effect, simple process and high recovery rate.
The specific implementation mode is as follows:
the following is a further description of the invention and is not intended to be limiting.
Example 1: method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution
The marine rare earth sulfuric acid leaching solution comprises the following components: rare earth ions (containing La, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, Y and Sc ions with the concentrations of 38.8, 5.7, 12, 52.6, 12.9, 3, 13.5, 2.2, 11.5, 2.5, 7, 1, 6, 0.9, 99 and 5.4mg/L respectively) 274mg/L and Fe 3+ 0.89g/L，Al 3+ 7.69g/L，Mn 2+ 1.12g/L，Mg 2+ 5.83g/L，Ca 2+ 0.55g/L. pH =0.68. 10% N1923, 10% TBP and 80% sulfonated kerosene by volume were prepared into the organic phase. Carrying out 3-stage countercurrent extraction on the marine rare earth sulfuric acid leaching solution and the extracted organic phase according to the ratio of 1.5 to 1.5, wherein the extraction time is 5min, the rare earth extraction rate is 97.21%, and the extraction rate is Fe 3+ The extraction rate is 100%, and other non-rare earth impurities are not extracted basically. Carrying out 1-stage back extraction on the rare earth-containing load organic phase by using 6mol/L hydrochloric acid according to a phase ratio (O/A) 1:1 for 10min, wherein the back extraction rate of rare earth is 98.93 percent, and Fe 3+ The rare earth is not substantially stripped to obtain separated rare earth stripping liquid; the rare earth recovery rate is calculated to be 96.17 percent.
Example 2: method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution
The marine rare earth sulfuric acid leaching solution comprises the following components: rare earth ions (containing La, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, Y and Sc ions with the concentrations of 38.8, 5.7, 12, 52.6, 12.9, 3, 13.5, 2.2, 11.5, 2.5, 7, 1, 6, 0.9, 99 and 5.4mg/L respectively) 274mg/L and Fe 3+ 0.89g/L，Al 3+ 7.69g/L，Mn 2+ 3.12g/L，Mg 2+ 5.83g/L，Ca 2+ 0.55g/L. pH =1.28. 10% N1923, 20% TBP and 70% sulfonated kerosene by volume were prepared as the organic phase. Performing 1-stage countercurrent extraction on the marine rare earth sulfuric acid leaching solution and the extracted organic phase according to the ratio of O/A of 1:1 for 10min, wherein the rare earth extraction rate is 95.13 percent, and Fe 3+ The extraction rate is 99.17%, and other non-rare earth impurities are not extracted basically. Carrying out 2-stage cross-flow back extraction on the rare earth-containing load organic phase by using 12mol/L hydrochloric acid according to a phase ratio (O/A) 2:1 for 10min, wherein the back extraction rate of the rare earth is 100 percent, and Fe 3+ The rare earth is not substantially stripped to obtain separated rare earth stripping liquid; the rare earth recovery rate is calculated to be 95.13%.
Example 3: method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution
The marine rare earth sulfuric acid leaching solution comprises the following components: rare earth ions (containing La, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, Y and Sc ions with the concentrations of 70, 10.3, 21.6, 94.7, 23.2, 5.4, 24.3, 3.9, 20.7, 4.5, 12.6, 1.8, 10.8, 1.6, 182.9 and 9.7mg/L respectively) 498mg/L Fe and 10.3 3+ 1.78g/L，Al 3+ 5.93g/L，Mn 2+ 3.71g/L，Mg 2+ 7.35g/L，Ca 2+ 0.62g/L。pH＝0.68。
30% N1923, 30% TBP and 40% sulfonated kerosene by volume were prepared into the organic phase. Performing 3-stage countercurrent extraction on the marine rare earth sulfuric acid leaching solution and the extracted organic phase according to the ratio of O/A of 1:2 for 10min, wherein the rare earth extraction rate is 98.22 percent, and Fe 3+ The extraction rate is 100%, and other non-rare earth impurities are not extracted basically.
Carrying out 3-stage countercurrent back extraction on the rare earth-containing load organic phase by using 9mol/L hydrochloric acid according to a phase ratio (O/A) 1:1 for 10min, wherein the back extraction rate of the rare earth is 100 percent, and Fe 3+ The rare earth is not substantially stripped to obtain separated rare earth stripping liquid; the rare earth recovery rate is calculated to be 98.22 percent.
Example 4: method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution
The marine rare earth sulfuric acid leaching solution comprises the following components: rare earth ions (containing La, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, Y and Sc ions with the concentrations of 70, 10.3, 21.6, 94.7, 23.2, 5.4, 24.3, 3.9, 20.7, 4.5, 12.6, 1.8, 10.8, 1.6, 182.9 and 9.7mg/L respectively) 498mg/L Fe and 10.3 3+ 1.78g/L，Al 3+ 5.93g/L，Mn 2+ 3.71g/L，Mg 2+ 7.35g/L，Ca 2+ 0.62g/L。pH＝0.25。
20% N1923, 20% TBP and 60% sulfonated kerosene by volume were prepared into the organic phase. Performing 3-stage cross-flow extraction on the marine rare earth sulfuric acid leaching solution and the extracted organic phase according to the ratio of O/A of 1:2 for 10min, wherein the rare earth extraction rate is 97.14 percent, and Fe 3+ The extraction rate is 100%, and other non-rare earth impurities are not extracted basically.
Carrying out 3-stage cross-flow back extraction on the rare earth-containing load organic phase by using 6mol/L hydrochloric acid according to a phase ratio (O/A) 1:1 for 10min, wherein the back extraction rate of the rare earth is 100 percent, and the Fe content is 3+ The rare earth is not substantially stripped to obtain separated rare earth stripping liquid; the rare earth recovery rate is calculated to be 97.14 percent.
Example 5: method for extracting and separating rare earth from marine rare earth sulfuric acid leaching solution
The marine rare earth sulfuric acid leaching solution comprises the following components: rare earth ions (containing La, ce, pr, nd, sm, eu, gd, tb, dy, ho, er, tm, yb, lu, Y and Sc ions with the concentrations of 70, 10.3, 21.6, 94.7, 23.2, 5.4, 24.3, 3.9, 20.7, 4.5, 12.6, 1.8, 10.8, 1.6, 182.9 and 9.7mg/L respectively) 498mg/L of Fe and 498mg/L of Fe 3+ 1.78g/L，Al 3+ 5.93g/L，Mn 2+ 3.71g/L，Mg 2+ 7.35g/L，Ca 2+ 0.62g/L。pH＝-0.5。
30% N1923, 30% TBP and 40% sulfonated kerosene by volume were prepared into the organic phase. Performing 3-stage cross-flow extraction on the marine rare earth sulfuric acid leaching solution and the extracted organic phase according to the ratio of O/A of 2:1 for 10min, wherein the rare earth extraction rate is 100 percent, and Fe 3+ The extraction rate is 100%, and other non-rare earth impurities are not extracted basically.
Carrying out 3-stage cross-flow back extraction on the rare earth-containing load organic phase by using 12mol/L hydrochloric acid according to a phase ratio (O/A) 1:1 for 5min, wherein the back extraction rate of the rare earth is 100 percent, and Fe 3+ The rare earth is not substantially stripped to obtain separated rare earth stripping liquid; the rare earth recovery rate is calculated to be 100%.
Comparative example 1: this comparative example is essentially the same as example 1 except that: the extracted organic phase was selected without adding TBP, 10% N1923 and 90% sulfonated kerosene by volume. Rare earth extraction rate of 92%, fe 3+ The extraction rate is 100%, al 3+ The extraction rate is 5.31 percent, and other non-rare earth impurities are not extracted basically. Rare earth metal saltThe extraction rate is 100 percent, fe 3+ The back extraction rate is 100 percent, and Al 3+ The back extraction rate is 100 percent, and the extraction separation of rare earth and non-rare earth impurities cannot be realized.
Comparative example 2: this comparative example is essentially the same as example 2, except that: the extracted organic phase was selected without the addition of N1923, 20% TBP +80% sulfonated kerosene by volume. Rare earth, fe 3+ And other non-rare earth impurities are not extracted, so that the extraction separation of rare earth and non-rare earth impurities cannot be realized.
Comparative example 3: this comparative example is essentially the same as example 3, except that: when the extraction organic phase is selected, N1923 and TBP are not added, and 100 percent of sulfonated kerosene is added according to the volume ratio. Rare earth, fe 3+ And other non-rare earth impurities are not extracted, so that the extraction separation of rare earth and non-rare earth impurities cannot be realized.
Comparative example 4: this comparative example is essentially the same as example 3, except that: the organic phase is extracted by replacing N1923 with N235, an extractant of the same type, by volume, 30% N235, 30% TBP and 40% sulfonated kerosene. Fe 3+ The extraction rate is 14.06 percent, the rare earth extraction rate is 1.27 percent, other non-rare earth impurities are not extracted basically, and the extraction separation of the rare earth and the non-rare earth impurities cannot be realized.
Comparative example 5: this comparative example is essentially the same as example 3, except that: the organic phase is extracted by replacing N1923 with the analogous extractant N263, 30% by volume N263, 30% by volume TBP and 40% by volume sulfonated kerosene. Fe 3+ The extraction rate is 8.54 percent, the extraction rate of the rare earth is 2.71 percent, other non-rare earth impurities are not extracted basically, and the extraction separation of the rare earth and the non-rare earth impurities cannot be realized.
Comparative example 6: this comparative example is essentially the same as example 4, except that: the organic phase is extracted by replacing TBP with the analogous extractant P350, 20% by volume N1923, 20% by volume P350 and 60% by volume sulfonated kerosene. Rare earth extraction rate 93.08%, fe 3+ The extraction rate is 100%, and other non-rare earth impurities are not extracted basically. The back extraction rate of rare earth is 100%, fe 3+ The back extraction rate is 71.58 percent, and the extraction separation of rare earth and non-rare earth impurities cannot be realized.
Comparative example 7: book (I)The comparative example is essentially the same as example 5 except that: extraction of the organic phase by replacement of N1923 with N235, and TBP with P350 as the same extractant, 30% N235, 30% P350 and 40% sulfonated kerosene. Fe 3+ 12.79 percent of extraction, 0.91 percent of rare earth extraction rate and no extraction of other non-rare earth impurities, thus the extraction separation of rare earth and non-rare earth impurities can not be realized.
Comparative example 8: this comparative example is essentially the same as example 5, except that: extraction of the organic phase by replacement of N1923 with N263, TBP with P350 as the same extractant, 30% N263, 30% P350 and 40% sulfonated kerosene. Fe 3+ The extraction rate is 5.96 percent, the extraction rate of the rare earth is 1.47 percent, other non-rare earth impurities are not extracted basically, and the extraction separation of the rare earth and the non-rare earth impurities cannot be realized.
Comparative example 9: this comparative example is essentially the same as example 1 except that: extraction of the organic phase by substituting N1923 with N235, the same extractant as N507, by 10% N235, 10% TBP, 10% P507 and 70% sulfonated kerosene. Fe 3+ The extraction rate is 33.12 percent, the rare earth extraction rate is 37.93 percent, other non-rare earth impurities are not extracted basically, the back extraction rate of the rare earth is 72.73 percent, and Fe 3+ The back extraction rate is 8.61%, and the extraction separation of rare earth and non-rare earth impurities cannot be realized.
By comparing the examples with the respective proportions, it can be seen that the extraction and separation effects on rare earth in the respective proportions are far inferior to those in the examples, and therefore, the fact that the mixed extraction of the organic phase by using the N1923-TBP-sulfonated kerosene for extracting and separating rare earth in the sulfuric acid system is not simple in extractant combination or similar substitution, and has an unexpected remarkable gain effect; and when the extraction mode, the stage number, the time and the like are in the range required by the application, the extraction rate and the separation recovery rate of the rare earth can be further ensured.
Claims (6)
1. A method for extracting and separating rare earth from a marine rare earth sulfuric acid leaching solution is characterized by comprising the following steps:
1) Extracting the ocean rare earth sulfuric acid leaching solution by adopting a secondary carbon primary amine extractant-tributyl phosphate-sulfonated kerosene mixed extractantObtaining a rare earth-containing load organic phase and a raffinate aqueous phase; wherein, the secondary carbon primary amine extractant-tributyl phosphate-sulfonated kerosene mixed extractant is prepared by the secondary carbon primary amine extractant, the tributyl phosphate and the sulfonated kerosene with the volume ratio of 1-3:1-3:4-8; the rare earth ion contained in the marine rare earth sulfuric acid leaching solution is 200-500 mg/L, fe 3+ 0.5～2g/L、Al 3+ 5～10g/L、Mn 2+ 1～5g/L、Mg 2+ 1 to 10g/L and Ca 2+ 0.5～1.0g/L；
2) And (2) carrying out back extraction on the rare earth-containing loaded organic phase obtained in the step 1) by using hydrochloric acid to obtain a separated rare earth back extraction solution.
2. The method as claimed in claim 1, wherein the extraction mode in step 1) is counter-current or cross-current extraction; the extraction phase ratio O/A is 1; the extraction stage number is 1-3; the extraction time is 5-10 min.
3. The method according to claim 1, wherein step 2) counter-current or cross-current stripping of hydrochloric acid is used for the rare earth-containing loaded organic phase; the back extraction phase ratio O/A is 1-2:1.
4. The method of claim 1, wherein the hydrochloric acid concentration is 6 to 12mol/L.
5. The method according to claim 1, wherein the stage number of the counter-current or cross-current back extraction in the step 2) is 1-3; the back extraction time is 5-10 min.
6. The method according to claim 1, wherein the marine rare earth sulfuric acid leach liquor pH = -0.5-1.5.
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