CN115505763A - Extraction method for improving praseodymium-neodymium output and controlling praseodymium content in praseodymium-neodymium - Google Patents
Extraction method for improving praseodymium-neodymium output and controlling praseodymium content in praseodymium-neodymium Download PDFInfo
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Abstract
The invention discloses an extraction method for improving the output of praseodymium-neodymium and controlling the praseodymium content in praseodymium-neodymium, which comprises the following steps: A. and setting rare earth extraction separation lines, wherein the rare earth extraction separation lines comprise a praseodymium dragging separation line, a praseodymium and neodymium dragging separation line, a samarium and europium and gadolinium dragging separation line and the like. According to the invention, the production status of an extraction working section is combined, an idle neodymium dragging and separating line is used as a praseodymium and neodymium dragging and separating line, and the original neodymium samarium extraction and separation line is used, so that the treatment capacity of a production line is increased under the condition of simply changing the existing neodymium samarium extraction and separation line, and further the daily yield of rare earth is improved.
Description
Technical Field
The invention relates to the technical field of rare earth extraction and separation, in particular to an extraction method for improving the output of praseodymium-neodymium and controlling the praseodymium-neodymium content.
Background
In the rare earth hydrometallurgy technology, the rare earth extraction separation technology is the key to obtaining various single rare earth products, and the praseodymium-neodymium product is used as a high-value rare earth product, and the design of a neodymium-samarium extraction separation line is particularly important. In the industry, the common design of the neodymium samarium extraction separation line is: the extraction and separation line with 72 stages of extraction tanks is formed by serially arranging extraction tanks (mixing clarifier structures) with the capacity of 100L, as shown in figure 2, the front 1-20 stages of the existing neodymium samarium extraction and separation line are rare earth soap sections, 21-40 stages are extraction sections, 41-56 stages are washing sections, and 57-72 stages are back extraction sections. Allowing a neodymium samarium feed liquid to enter from a 41 st level, allowing a 69 th level hydrochloric acid solution and a 1 st level to be saponified organically, producing a samarium europium gadolinium chloride feed liquid at a 57 th level, allowing a part of the samarium europium gadolinium chloride feed liquid to flow back, producing a praseodymium neodymium chloride feed liquid at a 21 st level, allowing a part of the praseodymium neodymium chloride feed liquid to flow back, discharging rare earth wastewater at the 1 st level, and discharging a blank organic material at the 72 th level. The prior neodymium samarium extraction separation line mainly has the following technical defects: 1. the treatment capacity cannot meet the requirement, the single-day rare earth yield is not more than 2.3t, and the yield is difficult to promote; 2. the praseodymium distribution in the praseodymium neodymium chloride feed liquid reaches 26-33w percent, which is higher than the praseodymium distribution of qualified products in the market by more than 3 percent (the praseodymium distribution of the qualified products is 23-27w percent), so expensive neodymium oxide needs to be added into the praseodymium neodymium chloride feed liquid to adjust the distribution, and the production cost is overhigh. Therefore, the existing neodymium samarium extraction separation line needs to be modified to overcome the existing problems.
Disclosure of Invention
The invention aims to: the invention provides an extraction method for improving the output of praseodymium and neodymium and controlling the praseodymium content in praseodymium and neodymium, which combines the current production situation of an extraction section, uses an idle dragging lanthanum separation line as a dragging praseodymium and neodymium separation line, and continues to use the original neodymium and samarium extraction separation line, increases the treatment capacity of a production line under the condition of simply changing the existing neodymium and samarium extraction separation line, further improves the daily output of rare earth, simultaneously controls praseodymium and neodymium distribution by using the original partial samarium extraction separation line as the dragging praseodymium separation line under the condition of not adding extra neodymium oxide, and also obtains a high-purity praseodymium product, and overcomes the defects of the existing neodymium and samarium extraction separation line.
The technical scheme adopted by the invention is as follows: an extraction method for improving the output of praseodymium-neodymium and controlling the praseodymium content in praseodymium-neodymium comprises the following steps:
A. the method comprises the following steps that rare earth extraction separation lines are arranged, wherein the rare earth extraction separation lines comprise a praseodymium dragging separation line, a praseodymium dragging neodymium separation line and a samarium europium gadolinium dragging separation line, the praseodymium dragging separation line comprises a rare earth soap section and an extraction section, the praseodymium dragging neodymium separation line comprises a rare earth soap section and an extraction section, the samarium dragging europium gadolinium separation line comprises a washing section and a back extraction section, and the praseodymium dragging separation line, the praseodymium dragging neodymium separation line and the samarium gadolinium dragging separation line are formed by serially connecting a plurality of stages of extraction grooves;
B. allowing the neodymium samarium feed liquid and the saponified organic material to enter a samarium-europium-gadolinium separation line, treating the neodymium samarium feed liquid and the saponified organic material through a washing section and a back extraction section to obtain a blank organic material and samarium-europium-gadolinium chloride feed liquid in the back extraction section, and refluxing part of the samarium-europium-gadolinium chloride feed liquid to a washing soap section for mixing and extraction to obtain a praseodymium-neodymium chloride solution;
C. the praseodymium neodymium chloride solution enters as the aqueous phase of the extraction section of the praseodymium neodymium fishing separation line, after the extraction section is treated, the praseodymium neodymium distributing qualified praseodymium neodymium chloride feed liquid is obtained, and the organic phase discharged from the praseodymium neodymium fishing separation line is used as the saponification organic of the samarium europium gadolinium fishing separation line; part of the obtained qualified praseodymium neodymium chloride feed liquid reflows to the rare earth soap section for mixed extraction to obtain a praseodymium chloride solution;
D. the praseodymium chloride solution enters as a water phase of the extraction section of the praseodymium-fishing separation line, saponified organic flows in from the rare earth soap section of the praseodymium-fishing separation line and flows out from the extraction section, praseodymium chloride feed liquid is obtained after treatment of the extraction section, the discharged organic phase is used as saponified organic of the praseodymium-fishing separation line, and part of the obtained praseodymium chloride feed liquid flows back to the rare earth soap section for mixed extraction, so that rare earth wastewater is obtained.
Further, the praseodymium-fishing separation line comprises 30-60 extraction grooves (for example, 30, 32, 33, 35, 40, 60, etc.), the praseodymium-fishing neodymium separation line comprises 20-40 extraction grooves (for example, 20, 22, 25, 26, 32, 40, etc.), and the samarium-europium-fishing gadolinium separation line comprises 20-40 extraction grooves (for example, 20, 22, 25, 30, 32, 40, etc.).
Furthermore, the praseodymium and neodymium dragging separation line consists of a rare earth soap section and an extraction section of the neodymium-samarium extraction separation line, the samarium-europium-gadolinium dragging separation line consists of a washing section and a back extraction section of the neodymium-samarium extraction separation line, and the praseodymium and neodymium dragging separation line consists of a lanthanum dragging separation line.
Furthermore, 72 grades of extraction tanks are connected in series with the neodymium-samarium extraction separation line, the front 40 grades of extraction tanks of the neodymium-samarium extraction separation line form a praseodymium dragging separation line, the rear 32 grades of the neodymium-samarium extraction separation line form a samarium-europium-gadolinium dragging separation line, and the extraction tanks connected in series with the lanthanum dragging separation line form 32 grades.
Further, the front 20 stages of extraction tanks of the neodymium-samarium extraction separation line are rare-earth soap sections, the rear 20 stages of extraction tanks are extraction sections, the 41 th to 56 th stages of extraction tanks of the neodymium-samarium extraction separation line are washing sections, and the 57 th to 69 th stages of extraction tanks are back-extraction sections; the front 11-stage extraction tank of the lanthanum dragging separation line is a rare earth soap section, and the rear 21-stage extraction tank is an extraction section.
Furthermore, the capacity of the single extraction tank of the lanthanum dragging separation line is larger than that of the single extraction tank of the neodymium samarium extraction separation line.
Further, neodymium-samarium feed liquid enters from a 41 th-level extraction tank of a neodymium-samarium extraction separation line, hydrochloric acid solution enters from a 69 th-level extraction tank of the neodymium-samarium extraction separation line, samarium-europium-gadolinium chloride feed liquid is discharged from a 57 th-level extraction tank of the neodymium-samarium extraction separation line, and part of samarium-europium-gadolinium chloride feed liquid reflows from a 56 th-level extraction tank to a 41 th-level discharge praseodymium-neodymium chloride solution; allowing the praseodymium-neodymium chloride solution to enter from a 32 th-level extraction tank for dragging a lanthanum separation line, allowing a praseodymium-neodymium chloride solution to be qualified and distributed from a 12 th-level extraction tank, allowing part of the praseodymium-neodymium chloride solution to flow back from a 11 th-level extraction tank, and discharging the praseodymium chloride solution to a 1 st-level extraction tank; the praseodymium chloride solution enters from the 40 th-level extraction tank of the praseodymium fishing separation line, qualified praseodymium chloride feed liquid is discharged from the 21 st-level extraction tank, part of the praseodymium chloride feed liquid flows back from the 20 th-level extraction tank, rare earth wastewater is discharged from the 1 st level, saponified organic matter enters from the 1 st-level extraction tank of the praseodymium fishing separation line and flows out from the 40 th-level extraction tank of the praseodymium fishing separation line.
Further, the reflux amount of samarium europium gadolinium chloride solution is 1/4-2/3 (for example, 1/4, 1/3, 1/2, 2/3, etc.) of the total amount; the reflux quantity of the praseodymium neodymium chloride feed liquid is 1/4-2/3 (for example, 1/4, 1/3, 1/2, 2/3, etc.) of the total quantity; the reflux amount of the praseodymium chloride solution is 1/4-2/3 (for example, 1/4, 1/3, 1/2, 2/3, etc.) of the total amount thereof.
Further, the feeding flow rate of the neodymium samarium feed liquid is 10 to 20L/s, and may be, for example, 10L/s, 12L/s, 13.4L/s, 13.8L/s, 14L/s, 15L/s, 20L/s, etc.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. according to the invention, the idle lanthanum fishing separation line is used as a praseodymium-neodymium fishing separation line, and the original neodymium-samarium extraction separation line is used, so that the treatment capacity of the production line is increased under the condition of simply changing the existing neodymium-samarium extraction separation line, the daily yield of rare earth is further improved, the daily yield is improved to be more than 3.0t from 2.3t, and the yield improvement effect is obvious;
2. according to the invention, the rare earth soap section and the extraction section of the original neodymium-samarium extraction separation line are used as the praseodymium dragging separation line, the existing lanthanum dragging separation line is used as the new rare earth soap section and the extraction section, and the original washing section and the back extraction section of the neodymium-samarium extraction separation line are unchanged.
Drawings
Fig. 1 is a schematic flow chart of an extraction method for improving the productivity of praseodymium and neodymium and controlling the praseodymium content in praseodymium and neodymium.
FIG. 2 is a schematic flow chart of the existing extraction and separation line of neodymium samarium.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings.
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is described in further detail below with reference to the accompanying drawings and embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in figure 1, an extraction method for improving the production of praseodymium-neodymium and controlling the praseodymium-neodymium content is characterized in that a 32-level lanthanum dragging extraction separation line is arranged between original 72-level neodymium-samarium extraction separation lines, the lanthanum dragging extraction separation line forms a praseodymium-neodymium extraction separation line, an extraction tank of the neodymium-samarium extraction separation line is an extraction tank with the capacity of 100L, an extraction tank of the lanthanum dragging extraction separation line is an extraction tank with the capacity of 400L, and the tank body structures of the two extraction lines are the same except for different sizes. Correspondingly, for the tank body structure of the extraction tank, the existing widely-used extraction tank with a typical mixing and clarifying structure comprising a mixing chamber and a clarifying chamber is adopted, and as the extraction tank belongs to the existing structure, the working principle of mixing and clarifying can be realized by referring to the prior art, and the details are not repeated.
Accordingly, the arrangement of the extraction tanks at different levels can be as follows, for example, the extraction tanks can be arranged in series to form a multi-stage extraction tank, and each stage of the extraction tank comprises a mixing chamber and a clarifying chamber. Meanwhile, it is worth to be noted that, the extraction tank is used for rare earth extraction, a rare earth solvent extraction separation technology is generally adopted, the technology is a mature technology widely adopted at present, the invention is not exceptional, and the technology is also used for rare earth extraction separation, and the separation principle of the technology can refer to the existing document of rare earth separation technical state analysis, han Qiying, hunan nonferrous metal, 2010.26 (1): 24-27.
Furthermore, the innovation of the present invention is that the original neodymium-samarium separation line is redesigned, as shown in fig. 1, neodymium-samarium feed liquid enters from the 41 st stage extraction tank of the neodymium-samarium extraction separation line as a water phase, and is mixed with saponified organic as an organic phase in the 41 st stage extraction tank, after multi-stage extraction (flowing direction is 41 st stage → 69 st stage), enters the 69 th stage extraction tank of the neodymium-samarium extraction separation line, 5.5mol/L hydrochloric acid feed liquid is added into the 69 th stage extraction tank of the neodymium-samarium extraction separation line for back extraction, so as to obtain blank organic and water phases, the blank organic samarium continues to flow backwards (flowing direction is 69 th stage → 72 th stage) until reaching the 72 th stage extraction tank of the neodymium-samarium extraction separation line, blank organic is discharged through an organic discharge port of the 72 th stage extraction tank, blank organic continues to be reused, the water phase of the 72 th stage extraction tank returns to the stage extraction tanks (flowing direction is 72 th stage → 57 st stage), and is mixed with the mixed phase in the extraction tanks, and when the mixed phase reaches the second stage extraction tank, organic phase is discharged through the gadolinium extraction tank, so as organic phase, so as to obtain organic chloride extraction liquid phase, and the organic phase is discharged through the gadolinium extraction tank, so as a final extraction liquid phase extracted by the gadolinium extraction tank. Because the mixed phase of the extraction tanks of 41 th to 56 th stages contains praseodymium neodymium, a part of samarium europium gadolinium chloride feed liquid enters from a water phase inlet of the extraction tank of 56 th stage as washing liquid, returns to the extraction tanks of 41 th to 56 th stages step by step (the flow direction is 56 th stage → 41 th stage), and is continuously mixed with the mixed phase in the extraction tanks in the flow process, praseodymium neodymium ions mixed with the organic phase in the mixed phase return to the water phase again, and samarium europium gadolinium ions in the water phase are saponified and are fished out again to enter the organic phase, so that the purpose of washing step by step is achieved, the circulation is carried out, the water phase from the extraction tank of 41 th stage of the neodymium extraction separation line is praseodymium neodymium chloride solution without samarium gadolinium ions, the extraction tank of 57 th stage is samarium gadolinium chloride feed liquid, and the organic phase from the extraction tank of 72 th stage is blank organic.
Further, because the praseodymium content in the obtained praseodymium-neodymium chloride solution is high and reaches 26-33w%, in order to adjust the praseodymium-neodymium distribution without adding expensive neodymium oxide, the invention utilizes the original idle lanthanum fishing extraction separation line as the praseodymium-neodymium fishing separation line, and the flow is as follows: the saponification organic phase enters from a 1 st-stage extraction tank of a lanthanum fishing extraction separation line and flows backwards to a 32 nd-stage extraction tank step by step (the organic phase flows to the 1 st stage → the 32 nd stage), the water phase from a 41 st-stage extraction tank of a neodymium-samarium extraction separation line enters into a 32 nd-stage extraction tank to be mixed and flows towards the 1 st-stage extraction tank step by step, the 1 st-11 th-stage extraction tank is a rare earth soap section, the 12 th-32 th-stage extraction tank is an extraction section, the 1 st-11 th-stage extraction tank mainly extracts neodymium ions from praseodymium neodymium chloride, praseodymium ions are remained in the water phase, the 12 th-32 th-stage extraction tank mainly back extracts the neodymium ions in the organic phase into the water phase, and then praseodymium chloride feed liquid neodymium is obtained, and the organic phase is used as the saponification organic phase of the neodymium-samarium extraction separation line. The praseodymium-neodymium chloride solution enters from a 32 th-level extraction tank of the lanthanum dragging extraction separation line and flows forwards to a 12 th-level extraction tank, so that a praseodymium-neodymium partition qualified praseodymium-neodymium chloride feed liquid is obtained, and a praseodymium-neodymium chloride product is obtained. Correspondingly, one part of qualified praseodymium-neodymium chloride feed liquid is output as a product, the other part of praseodymium-neodymium chloride feed liquid is used as a rare earth soap material to be mixed and extracted with saponification organic, the rare earth soap material enters from a level-11 extraction tank of the lanthanum fishing extraction separation line and is mixed with the rare earth soap in the level-11 extraction tank, neodymium ions in the rare earth soap material continuously enter an organic phase by utilizing the characteristic of praseodymium-neodymium partition difference, praseodymium ions in the organic phase enter an aqueous phase (saponification organic preferential neodymium fishing), when the aqueous phase reaches the level-1 of the lanthanum fishing extraction separation line, the discharged aqueous phase is a praseodymium chloride solution, and the organic phase flows backwards, so that the purpose of praseodymium fishing is achieved.
The saponification organic entering the lanthanum fishing and extracting separation line is the saponification organic discharged from the praseodymium fishing and extracting separation line, the praseodymium fishing and extracting separation line is composed of 1 st-40 th-stage extraction groove sections of the original neodymium-samarium extracting and separating line, the blank organic is saponified by adding alkali to obtain the saponification organic, the saponification organic enters from the 1 st-stage extraction groove of the praseodymium fishing and extracting separation line and then flows to the 40 th-stage extraction groove of the praseodymium fishing and extracting separation line step by step, the praseodymium fishing and extracting separation line is also divided into a rare earth soap section (1 st-20 th-stage extraction groove) and an extraction section (21 st-40 th-stage extraction groove), the praseodymium chloride solution discharged from the 1 st-stage extraction groove of the lanthanum fishing and separating line enters from the 40 th-stage extraction groove of the praseodymium fishing and extracting and separating line and flows to the 1 st-stage extraction groove of the praseodymium fishing and extracting separation line, the praseodymium chloride solution is mixed with the saponification organic step by step in the praseodymium fishing and extracting separation line, and the 21 st-stage extraction groove of the praseodymium chloride solution is used as a chloride material liquid which can be recycled. Correspondingly, in order to keep the water phase balance of the praseodymium-fishing extraction separation line, a part of praseodymium chloride feed liquid from the 21 st-stage extraction tank needs to enter the praseodymium-fishing extraction separation line again, namely a part of praseodymium chloride feed liquid is used as rare earth soap material, enters from the 20 th stage of the praseodymium-fishing extraction separation line and then flows out from the 1 st-stage extraction tank, in the 1 st-20 th-stage rare earth soap section of the praseodymium-fishing extraction separation line, praseodymium is continuously fished out from the praseodymium chloride feed liquid by saponification organic, then praseodymium chloride is released from the extraction section (21 st-40 th stage), the water phase discharged from the 1 st-stage extraction tank of the rare earth soap section is rare earth wastewater without rare earth (praseodymium and neodymium), and the rare earth soap can directly enter a wastewater treatment station for treatment, and after the rare earth soap discharged from the 20 th-stage extraction tank is extracted by the extraction section, the discharged organic phase is used as saponification organic for the lanthanum-fishing separation line.
The invention relates to an extraction method for improving the production quantity of praseodymium-neodymium and controlling the praseodymium-neodymium content, which is characterized in that on the basis of combining the existing neodymium-samarium extraction separation line, in order to achieve the purposes of improving the treatment quantity and controlling the praseodymium-neodymium proportion ratio, an original idle lanthanum fishing extraction separation line is added in the middle section of an extraction groove of the original neodymium-samarium extraction separation line, so that the neodymium-samarium extraction separation line is composed of 3 sections of extraction separation lines, the front section (the 1 st to 40 th grade extraction grooves of the original neodymium-samarium extraction separation line) is the praseodymium fishing extraction separation line to produce praseodymium chloride products, the lanthanum fishing extraction separation line (the 1 st to 32 th grade extraction grooves) in the middle section is the praseodymium-neodymium fishing separation line to produce neodymium chloride products, and the rear section (the 41 st to 72 th grade extraction grooves of the original neodymium-samarium extraction separation line) is the samarium-gadolinium separation line to produce samarium-gadolinium chloride products. Therefore, the yield of the original 72-grade neodymium samarium extraction separation line is improved from 2.3t/d REO (rare earth amount) to more than 3t/d REO (rare earth amount), the treatment capacity is obviously improved, a praseodymium-neodymium chloride product with 23-27% of praseodymium content can be obtained, neodymium oxide does not need to be additionally added to adjust praseodymium-neodymium partition, a high praseodymium product with the purity of more than 99.5% can be obtained, the problems that the treatment capacity of the existing neodymium samarium extraction separation line is small, and expensive neodymium oxide needs to be added to adjust praseodymium-neodymium partition are solved, and the praseodymium content in the praseodymium-neodymium product is controlled.
To better illustrate the innovations of the present invention, the following examples are listed:
example 1
Taking the rare earth extraction separation line shown in fig. 1 as an example, the front section of the rare earth extraction separation line is a praseodymium fishing separation line, which is composed of 1-40 stages of extraction grooves of the original neodymium-samarium extraction separation line, the middle section is a praseodymium-neodymium fishing separation line, which is composed of 1-32 stages of extraction grooves lanthanum fishing separation lines left unused originally, the rear section is a samarium-gadolinium fishing separation line, which is composed of 41-72 stages of extraction grooves of the original neodymium-samarium extraction separation line, the 41 th stage of extraction groove of the rear section feeds neodymium-samarium feed liquid, wherein the praseodymium-neodymium concentration of the neodymium-samarium feed liquid is 233.5g/L, samarium-gadolinium concentration is 233.88g/L, the feed flow rate is 13.4L/s, the 69 th stage of extraction groove feeds-hydrochloric acid feed liquid with concentration of 5.5mol/L, the feed flow rate is 2.18L/min, the 57 th stage outputs samarium-gadolinium chloride feed liquid, wherein the samarium-gadolinium concentration is 233.88g/L, the samarium-gadolinium concentration is 3425 g/L, and the europium-gadolinium is recycled. And (2) allowing 1/3 of the total amount of samarium-europium-gadolinium chloride solution to enter from the 56 th-level extraction tank and reflux, allowing the water phase produced at the 41 th-level extraction tank to directly enter the 32 th-level extraction tank of the praseodymium-neodymium separation line, and allowing the organic phase produced at the 32 nd-level extraction tank of the praseodymium-neodymium separation line to directly enter the 41 th-level extraction tank of the samarium-europium-gadolinium separation line. In the praseodymium neodymium chloride produced by the 12 th grade of the praseodymium neodymium fishing separation line, the praseodymium partition is about 24w percent. And (3) allowing a 1/3 total amount of the praseodymium-neodymium chloride solution to enter the 11 th-level extraction tank and reflux, allowing the aqueous phase discharged from the 1 st-level extraction tank to directly enter the 40 th-level extraction tank of the praseodymium-dragging separation line, and allowing the organic phase discharged from the 40 th-level extraction tank of the praseodymium-neodymium dragging separation line to enter the 1 st-level extraction tank of the praseodymium-neodymium dragging separation line. The rare earth content in the rare earth wastewater discharged from the 1 st-stage extraction tank of the praseodymium collection separation line is 0.005g/L, the rare earth loss rate is within a controllable range, the praseodymium concentration in the praseodymium chloride feed liquid discharged from the 21 st-stage extraction tank is 235.29g/L, the praseodymium chloride feed liquid is treated by carbon precipitation and the like to obtain praseodymium oxide, and the praseodymium oxide purity is 99.5 percent. The yield of the rare earth extraction separation line is 3.0t/d REO.
Example 2
Example 2 is substantially the same as example 1 except that the neodymium samarium feed solution has a praseodymium-neodymium concentration of 235.29g/L and a samarium-europium-gadolinium concentration of 233.88g/L. The production result is as follows: in the produced samarium-europium-gadolinium chloride feed liquid, the concentration of samarium-europium-gadolinium is 219.51g/L, and the concentration of praseodymium-neodymium is 235.29g/L; in the produced praseodymium neodymium chloride, the distribution of praseodymium is about 24w%; in the produced praseodymium chloride feed liquid, the praseodymium concentration is 234.5g/L, and the praseodymium oxide purity is 99.7 percent; in the discharged rare earth wastewater, the rare earth concentration is 0.005g/L, and the single-day rare earth yield REO is 3.15t.
Example 3
Example 3 is substantially the same as example 1, except that the samarium neodymium feed solution has a praseodymium neodymium concentration of 233.5g/L and a samarium europium gadolinium concentration of 233.88g/L. The production result is as follows: in the produced samarium-europium-gadolinium chloride feed liquid, the concentration of samarium-europium-gadolinium is 219.51g/L, and the concentration of praseodymium-neodymium is 235.29g/L; in the produced praseodymium neodymium chloride, the distribution of praseodymium is about 24w%; in the produced praseodymium chloride feed liquid, the praseodymium concentration is 234.5g/L, and the praseodymium oxide purity is 99.65%; in the discharged rare earth wastewater, the rare earth concentration is 0.005g/L, and the single-day rare earth yield REO is 3.1t.
Comparative example 1
Comparative example 1 is essentially the same as example 1 except that the original 72 stage neodymium samarium extraction separation line was used, the process flow is shown in fig. 2, and the conditions were otherwise the same (e.g., the same concentration of neodymium samarium feed solution was used). The production result is as follows: in the produced samarium-europium-gadolinium chloride feed liquid, the concentration of samarium-europium-gadolinium is 233.88g/L, and the concentration of praseodymium-neodymium is 233.50g/L; in the produced praseodymium neodymium chloride, the praseodymium distribution is about 28w percent and is higher than the praseodymium distribution requirement in the market, and neodymium oxide needs to be mixed to reduce the praseodymium distribution; in the discharged rare earth wastewater, the rare earth concentration is 0.005g/L, and the single-day rare earth yield REO is 2.3t.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (9)
1. An extraction method for improving the output of praseodymium-neodymium and controlling the praseodymium content in the praseodymium-neodymium is characterized by comprising the following steps:
A. the method comprises the following steps that rare earth extraction separation lines are arranged, wherein each rare earth extraction separation line comprises a praseodymium fishing separation line, a praseodymium fishing neodymium separation line and a samarium fishing europium gadolinium separation line, each praseodymium fishing separation line comprises a rare earth soap section and an extraction section, each praseodymium fishing neodymium separation line comprises a rare earth soap section and an extraction section, each samarium fishing europium gadolinium separation line comprises a washing section and a back extraction section, and each praseodymium fishing separation line, each praseodymium fishing neodymium separation line and each samarium fishing gadolinium separation line are formed by serially connecting multi-stage extraction grooves;
B. allowing the neodymium samarium feed liquid and the saponified organic samarium-europium-gadolinium inlet fishing line to be treated by a washing section and a back extraction section, obtaining blank organic and samarium-europium-gadolinium chloride feed liquid in the back extraction section, and refluxing part of the samarium-europium-gadolinium chloride feed liquid to a washing soap section for mixing and extraction to obtain praseodymium-neodymium chloride solution;
C. the praseodymium-neodymium chloride solution enters as the aqueous phase of the extraction section of the praseodymium-neodymium fishing separation line, after the extraction section is processed, a praseodymium-neodymium distribution qualified praseodymium-neodymium feed liquid is obtained, and the organic phase discharged from the praseodymium-neodymium fishing separation line is used as saponification of samarium-europium-gadolinium separation lines; part of the obtained qualified praseodymium neodymium chloride feed liquid reflows to the rare earth soap section for mixed extraction to obtain a praseodymium chloride solution;
D. the praseodymium chloride solution enters as a water phase of the extraction section of the praseodymium-fishing separation line, saponified organic flows in from the rare earth soap section of the praseodymium-fishing separation line and flows out from the extraction section, praseodymium chloride feed liquid is obtained after treatment of the extraction section, the discharged organic phase is used as saponified organic of the praseodymium-fishing separation line, and part of the obtained praseodymium chloride feed liquid flows back to the rare earth soap section for mixed extraction, so that rare earth wastewater is obtained.
2. The extraction method for improving the praseodymium-neodymium output and controlling the praseodymium content in the praseodymium-neodymium component according to claim 1, wherein the praseodymium-dragging separation line comprises 30-60 grade extraction grooves, the praseodymium-neodymium dragging separation line comprises 20-40 grade extraction grooves, and the samarium-europium-gadolinium dragging separation line comprises 20-40 grade extraction grooves.
3. The extraction method for improving the praseodymium-neodymium output and controlling the praseodymium-neodymium content is characterized in that the praseodymium-dragging separation line is composed of a rare earth soap section and an extraction section of a neodymium-samarium extraction separation line, the samarium-europium-gadolinium dragging separation line is composed of a washing section and a back extraction section of the neodymium-samarium extraction separation line, and the praseodymium-neodymium dragging separation line is composed of a lanthanum dragging separation line.
4. The extraction method for improving the productivity of praseodymium-neodymium and controlling the praseodymium content in praseodymium-neodymium according to claim 3, wherein the neodymium-samarium extraction separation lines are connected in series by 72 stages of extraction tanks, the first 40 stages of extraction tanks of the neodymium-samarium extraction separation lines form praseodymium fishing separation lines, the last 32 stages of the neodymium-samarium extraction separation lines form samarium-europium-gadolinium fishing separation lines, and the lanthanum-fishing separation lines are connected in series by 32 stages of extraction tanks.
5. The extraction method for improving the production of praseodymium-neodymium and controlling the praseodymium content in praseodymium-neodymium according to claim 4, wherein the first 20 stages of extraction tanks of the neodymium-samarium extraction separation line are rare earth soap sections, the last 20 stages of extraction tanks are extraction sections, the 41 th to 56 th stages of extraction tanks of the neodymium-samarium extraction separation line are washing sections, and the 57 th to 69 th stages of extraction tanks are back extraction sections; the front 11-stage extraction tank of the lanthanum dragging separation line is a rare earth soap section, and the rear 21-stage extraction tank is an extraction section.
6. The extraction method for improving the productivity of praseodymium-neodymium and controlling the praseodymium content in praseodymium-neodymium according to claim 5, wherein the capacity of the single extraction tank of the lanthanum dragging separation line is larger than the capacity of the single extraction tank of the neodymium-samarium extraction separation line.
7. The method of claim 6, wherein the neodymium-neodymium feed liquid enters from the 41 st stage extraction tank of the neodymium-samarium extraction separation line, the hydrochloric acid solution enters from the 69 th stage extraction tank of the neodymium-samarium extraction separation line, the 57 th stage extraction tank of the neodymium-samarium extraction separation line discharges samarium-europium-gadolinium chloride feed liquid, and part of the samarium-europium-gadolinium chloride feed liquid flows back from the 56 th stage extraction tank to the 41 th stage discharge praseodymium-neodymium chloride solution; allowing the praseodymium-neodymium chloride solution to enter from a 32 th-level extraction tank of the lanthanum fishing separation line, allowing part of the praseodymium-neodymium chloride solution to flow back from a 11 th-level extraction tank from the praseodymium-neodymium chloride solution which is qualified and distributed from a 12 th-level extraction tank, and discharging the praseodymium chloride solution from a 1 st-level extraction tank; the praseodymium chloride solution enters from the 40 th-level extraction tank of the praseodymium fishing separation line, qualified praseodymium chloride feed liquid is discharged from the 21 st-level extraction tank, part of the praseodymium chloride feed liquid flows back from the 20 th-level extraction tank, rare earth wastewater is discharged from the 1 st level, saponified organic matter enters from the 1 st-level extraction tank of the praseodymium fishing separation line and flows out from the 40 th-level extraction tank of the praseodymium fishing separation line.
8. The extraction method for improving the praseodymium-neodymium yield and controlling the praseodymium content in praseodymium-neodymium according to claim 7, characterized in that the reflux amount of samarium gadolinium chloride feed liquid is 1/4-2/3 of its total amount; the reflux quantity of the praseodymium neodymium chloride feed liquid is 1/4-2/3 of the total quantity of the praseodymium neodymium chloride feed liquid; the reflux amount of the praseodymium chloride feed liquid is 1/4-2/3 of the total amount of the praseodymium chloride feed liquid.
9. The extraction method for improving the praseodymium-neodymium output and controlling the praseodymium content in the praseodymium-neodymium according to claim 1, wherein the feeding flow rate of the neodymium-samarium material liquid is 10-20L/s.
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