CN115505763B - Extraction method for improving praseodymium and neodymium output and controlling praseodymium content in praseodymium and neodymium - Google Patents
Extraction method for improving praseodymium and neodymium output and controlling praseodymium content in praseodymium and neodymium Download PDFInfo
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Abstract
The invention discloses an extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium, which comprises the following steps: A. setting a rare earth extraction separation line, wherein the rare earth extraction separation line comprises a praseodymium and neodymium separation line, a samarium and europium separation line and the like. According to the invention, the idle separation line of the extracted lanthanum is taken as the separation line of the extracted praseodymium and neodymium, and the original separation line of the extracted samarium of neodymium is used, so that the processing capacity of the production line is increased under the condition of simply changing the existing separation line of the extracted samarium of neodymium, and the daily yield of rare earth is further improved.
Description
Technical Field
The invention relates to the technical field of rare earth extraction separation, in particular to an extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium.
Background
In rare earth hydrometallurgy, rare earth extraction separation technology is key to obtaining various single rare earth products, and praseodymium and neodymium products are used as high-value rare earth products, and design of neodymium and samarium extraction separation lines is particularly important. In the industry, the common design of neodymium samarium extraction separation lines is: the extraction separation line with 72 stages of extraction tanks is formed by serially arranging 100L of extraction tanks (mixer-settler structure), and as shown in figure 2, the front 1-20 stages of the existing neodymium samarium extraction separation line are rare earth soap stages, the 21 st-40 stages are extraction stages, the 41 st-56 stages are washing stages, and the 57 th-72 stages are back extraction stages. The neodymium samarium feed liquid enters from the 41 st stage, 69 th stage enters hydrochloric acid solution, 1 st stage enters saponification organic matter, samarium europium chloride gadolinium feed liquid is produced at the 57 th stage, samarium europium chloride gadolinium feed liquid partially flows back, praseodymium neodymium chloride feed liquid is produced at the 21 st stage, praseodymium neodymium chloride feed liquid partially flows back, rare earth wastewater is discharged at the 1 st stage, and blank organic matter is discharged at the 72 th stage. The existing neodymium samarium extraction separation line mainly has the following technical defects at present: 1. the processing capacity can not keep up with the demand, the single-day rare earth yield is not more than 2.3t, and the yield is difficult to be improved; 2. the praseodymium distribution in the praseodymium and neodymium chloride feed liquid is 26-33w percent, which is more than 3 percent higher than the praseodymium distribution of qualified products in the market (the praseodymium distribution of qualified products is 23-27w percent), so that expensive neodymium oxide needs to be added into the praseodymium and neodymium chloride feed liquid to adjust the distribution, and the production cost is too high. Therefore, it is needed to modify the existing separation line of neodymium-samarium extraction to overcome the existing problems.
Disclosure of Invention
The invention aims at: aiming at the problems, the invention provides an extraction method for improving the output of praseodymium and neodymium and controlling the praseodymium content in the praseodymium and neodymium, which combines the current production situation of an extraction working section, takes an idle separation line of taking lanthanum as a separation line of taking praseodymium and neodymium, and takes the original separation line of extracting samarium, under the condition of simply changing the existing separation line of extracting samarium, the processing capacity of the production line is increased, and further the daily output of rare earth is improved.
The technical scheme adopted by the invention is as follows: an extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in the praseodymium and neodymium comprises the following steps:
A. setting a rare earth extraction separation line, wherein the rare earth extraction separation line comprises a praseodymium-dragging separation line, a praseodymium-dragging separation line and a samarium-europium-gadolinium separation line, the praseodymium-dragging separation line comprises a rare earth soap section and an extraction section, the praseodymium-dragging-europium-gadolinium separation line comprises a washing section and a back extraction section, and the praseodymium-dragging separation line, the praseodymium-dragging separation line and the samarium-europium-gadolinium separation line are all formed by serially connecting multiple extraction tanks;
B. the method comprises the steps of (1) carrying out treatment on a neodymium-samarium feed liquid and a saponified organic feeding and fishing samarium-europium-gadolinium separation line through a washing section and a back extraction section to obtain blank organic and samarium-europium-gadolinium chloride feed liquid in the back extraction section, and carrying out mixed extraction on part of samarium-europium-gadolinium chloride feed liquid after refluxing to a washing soap section to obtain praseodymium-neodymium chloride solution;
C. the praseodymium and neodymium chloride solution enters as a water phase of an extraction section of a separation line of the praseodymium and neodymium, and is treated by the extraction section to obtain praseodymium and neodymium chloride feed liquid with qualified praseodymium and neodymium distribution, and an organic phase discharged from the separation line of the praseodymium and neodymium is used as a saponification organic phase of the separation line of the samarium and europium; partially refluxing the obtained qualified praseodymium chloride neodymium feed liquid to a rare earth soap section for mixed extraction to obtain praseodymium chloride solution;
D. the method comprises the steps of taking praseodymium chloride solution as a water phase of an extraction section of a praseodymium scooping separation line, allowing saponified organic to flow in from the rare earth soap section of the praseodymium scooping separation line, allowing the saponified organic to flow out from the extraction section, processing the liquid by the extraction section to obtain praseodymium chloride feed liquid, taking the discharged organic phase as a saponified organic phase of the praseodymium scooping separation line, and allowing the obtained praseodymium chloride feed liquid to partially flow back to the rare earth soap section for mixed extraction to obtain rare earth wastewater.
Further, the praseodymium and neodymium separation line comprises 30-60 extraction tanks (for example, 30, 32, 33, 35, 40, 60, etc.), the praseodymium and neodymium separation line comprises 20-40 extraction tanks (for example, 20, 22, 25, 26, 32, 40, etc.), and the samarium and europium and gadolinium separation line comprises 20-40 extraction tanks (for example, 20, 22, 25, 30, 32, 40, etc.).
Further, 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 separation line is composed of a washing section and a back extraction section of the neodymium-samarium extraction separation line, and the praseodymium-dragging neodymium separation line is composed of a lanthanum-dragging separation line.
Further, the extraction tanks connected in series with the neodymium samarium extraction separation line are 72 stages in total, the first 40 stages of extraction tanks of the neodymium samarium extraction separation line form a praseodymium-fishing separation line, the last 32 stages of the neodymium samarium extraction separation line form a samarium-europium-gadolinium separation line, and the extraction tanks connected in series with the lanthanum-fishing separation line are 32 stages in total.
Further, the first 20-stage extraction tank of the neodymium samarium extraction separation line is a rare earth soap section, the second 20-stage extraction tank is an extraction section, the 41-56-stage extraction tank of the neodymium samarium extraction separation line is a washing section, and the 57-69-stage extraction tank is a back extraction section; the first 11-stage extraction tank of the lanthanum fishing separation line is a rare earth soap section, and the second 21-stage extraction tank is an extraction section.
Further, the capacity of the single extraction tank of the lanthanum fishing separation line is larger than that of the single extraction tank of the neodymium samarium extraction separation line.
Further, the neodymium samarium feed liquid enters from a 41 st extraction tank of a neodymium samarium extraction separation line, the hydrochloric acid solution enters from a 69 th extraction tank of the neodymium samarium extraction separation line, the 57 th extraction tank of the neodymium samarium extraction separation line discharges samarium europium chloride gadolinium feed liquid, part of samarium europium chloride gadolinium feed liquid flows back from a 56 th extraction tank, and the praseodymium neodymium chloride solution is discharged from the 41 st extraction tank; the praseodymium neodymium chloride solution enters from a 32 th extraction tank of a lanthanum fishing separation line, the praseodymium neodymium chloride solution is qualified and distributed from a 12 th extraction tank, part of the praseodymium neodymium chloride solution flows back from an 11 th extraction tank to a 1 st extraction tank, and the praseodymium chloride solution is discharged; the praseodymium chloride solution enters from a 40 th extraction tank of the praseodymium scooping separation line, the qualified praseodymium chloride feed liquid is discharged from a 21 st extraction tank, part of the praseodymium chloride feed liquid flows back from a 20 th extraction tank, the rare earth wastewater is discharged from a 1 st extraction tank of the praseodymium scooping separation line, and saponified organic enters from the 40 th extraction tank of the praseodymium scooping separation line.
Further, the reflux amount of the samarium europium chloride gadolinium liquid is 1/4-2/3 (for example, 1/4, 1/3, 1/2, 2/3, etc.) of the total amount of the samarium europium chloride gadolinium liquid; the reflux amount of praseodymium chloride neodymium feed liquid is 1/4-2/3 of the total amount (for example, 1/4, 1/3, 1/2, 2/3, etc.); the reflux amount of praseodymium chloride feed liquid 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 liquid is 10-20L/s, for example, 10L/s, 12L/s, 13.4L/s, 13.8L/s, 14L/s, 15L/s, 20L/s and the like can be used.
In summary, due to the adoption of the technical scheme, the beneficial effects of the invention are as follows:
1. according to the invention, the idle separation line of the lanthanum is taken as the separation line of the praseodymium and neodymium, and the original separation line of the neodymium and samarium extraction is used, so that the processing capacity of the production line is increased under the condition of simply changing the existing separation line of the neodymium and samarium extraction, the daily yield of rare earth is further improved, the daily yield is improved from 2.3t to more than 3.0t, and the yield improving 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-fishing separation line, the existing lanthanum-fishing separation line is used as the new rare earth soap section and the extraction section, the original washing section and the back extraction section of the neodymium samarium extraction separation line are unchanged, so that the praseodymium-neodymium distribution in the praseodymium-neodymium chloride feed liquid can be controlled under the condition that no additional neodymium oxide is added, a praseodymium-neodymium product with qualified praseodymium-neodymium distribution can be living out, meanwhile, the setting of the praseodymium-fishing separation line also obtains a high-purity praseodymium product, the profit of enterprises is increased, and the defects of the existing neodymium-samarium extraction separation line are overcome.
Drawings
Fig. 1 is a schematic flow chart of an extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium in the invention.
Fig. 2 is a schematic diagram of a flow chart of a prior art separation line for neodymium samarium extraction.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
The present invention will be described in further detail with reference to the drawings and examples, in order to make the objects, technical solutions and advantages of the present invention more apparent. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
As shown in FIG. 1, an extraction method for improving the output of praseodymium and neodymium and controlling the praseodymium content in the praseodymium and neodymium is characterized in that a 32-level lanthanum-scooping extraction separation line is arranged between original 72-level neodymium and samarium extraction separation lines, the lanthanum-scooping extraction separation line forms a praseodymium and neodymium-scooping separation line, an extraction tank of the neodymium and samarium extraction separation line is an extraction tank with the capacity of 100L, an extraction tank of the lanthanum-scooping extraction separation line is an extraction tank with the capacity of 400L, and the tank structures of the two extraction tanks are identical except the sizes. Correspondingly, for the tank body structure of the extraction tank, the extraction tank with the typical mixing and clarifying structure comprising the mixing chamber and the clarifying chamber which are widely used in the prior art is adopted, and the working principle of mixing and clarifying of the extraction tank belongs to the prior art, so that the description is omitted.
Correspondingly, the arrangement mode of the extraction tanks at each stage is just to refer to the prior art, for example, the extraction tanks can be arranged in series to form a multi-stage extraction tank, and each stage of extraction tank comprises a mixing chamber and a clarifying chamber. Meanwhile, it is worth to say that, rare earth extraction is performed by using the extraction tank, generally, rare earth solvent extraction separation technology is adopted, which is a mature technology widely adopted at present, the invention is not exceptional, rare earth extraction separation is realized by adopting the technology, and the separation principle of the technology can be referred to the existing literature of rare earth separation technology state of the art analysis, han Qiying, hunan nonferrous metal, 2010.26 (1): 24-27.
Further, the invention is innovative in that the original neodymium samarium separation line is redesigned, as shown in fig. 1, the neodymium samarium liquid enters from the 41 st extraction tank of the neodymium samarium extraction separation line as an aqueous phase, is mixed with saponified organic serving as an organic phase in the 41 st extraction tank, after multistage extraction (the flow direction is the 41 st to 69 th), enters the 69 th extraction tank of the neodymium samarium extraction tank, 5.5mol/L hydrochloric acid liquid is added into the 69 th extraction tank of the neodymium samarium extraction separation line for back extraction, so as to obtain blank organic and aqueous phase, the blank organic continues to flow backwards (the flow direction is the 69 th to 72 th) until reaching the 72 nd extraction tank of the neodymium samarium extraction separation line, the blank organic is discharged through an organic discharge port of the 72 nd extraction tank, the aqueous phase of the 72 nd extraction tank is returned to the extraction tank (the flow direction is the 72 nd to 57 th) stage, and is mixed with the mixed phase in the extraction tank of each stage extraction tank and back extracted until reaching the 57 th extraction tank, and the blank organic phase is discharged to the aqueous phase through the gadolinium organic phase of the gadolinium extraction tank, so as to obtain the final blank organic liquid, namely the blank organic liquid is discharged from the gadolinium extraction tank through the stage of the gadolinium extraction tank. As the mixed phase of the extraction tank of the 41 th-56 th level contains praseodymium and neodymium, a part of samarium europium gadolinium chloride feed liquid is taken as washing liquid to enter from the water phase inlet of the extraction tank of the 56 th level, returns to the 41 th-56 th level step by step (the flow direction is 56 th level to 41 st level), is continuously mixed with the mixed phase in the extraction tank in the flowing process, praseodymium and neodymium ions in the organic phase in the mixed phase are mixed at the moment and return to the water phase again, samarium europium gadolinium ions in the water phase are fished out again by saponified organic matters and enter the organic phase, so that the aim of washing step by step is fulfilled, the water phase from the 41 st level extraction tank of the neodymium and samarium extraction separation line is praseodymium neodymium chloride solution without samarium europium gadolinium ions, the 57 th level extraction tank is the samarium europium gadolinium chloride feed liquid, and the organic phase from the 72 th extraction tank is blank organic.
Further, as the praseodymium content in the obtained praseodymium and neodymium chloride solution is higher and reaches 26-33w%, in order to adjust the praseodymium and neodymium distribution without adding expensive neodymium oxide, the invention uses the original idle separation line for extracting the lanthanum as the separation line for extracting the praseodymium and neodymium, and the flow is as follows: the saponification organic matter enters from the 1 st extraction tank of the lanthanum-fishing extraction separation line, flows backward to the 32 nd extraction tank step by step (the flow direction of the organic phase is 1 st to 32 nd), the water phase from the 41 st extraction tank of the neodymium-samarium extraction separation line enters into the 32 nd extraction tank for mixing, and flows forward to the 1 st extraction tank step by step, the 1 st to 11 th extraction tanks are rare earth soap sections, the 12 th to 32 th extraction tanks are extraction sections, the 1 st to 11 th extraction tanks mainly extract neodymium ions from praseodymium neodymium chloride, the praseodymium ions remain in the water phase, the 12 th to 32 nd extraction tanks mainly strip the neodymium ions in the organic phase into the water phase, thus obtaining praseodymium chloride feed liquid, and the organic phase is used as the saponification organic matter of the neodymium-samarium extraction separation line. And (3) entering the praseodymium and neodymium chloride solution from a 32 th extraction tank of a lanthanum fishing extraction separation line, and when the solution flows forward to a 12 th extraction tank, obtaining praseodymium and neodymium chloride feed liquid with qualified praseodymium and neodymium components, thereby obtaining a praseodymium and neodymium chloride product. Correspondingly, a part of qualified praseodymium and neodymium chloride feed liquid is output as a product, the other part of the praseodymium and neodymium chloride feed liquid is used as a rare earth soap material to be mixed and extracted with saponifying organic, the rare earth soap material enters from an 11 th extraction tank of a lanthanum-fishing extraction separation line and is mixed with rare earth soap in the 11 th extraction tank, by utilizing the characteristic of poor praseodymium and neodymium distribution at the moment, neodymium ions in the rare earth soap material continuously enter an organic phase, praseodymium ions in the organic phase enter an aqueous phase (the saponifying organic preferentially drags neodymium), and when the aqueous phase reaches the 1 st stage of the lanthanum-fishing extraction separation line, the discharged aqueous phase is praseodymium chloride solution, and the organic phase flows backwards, thereby achieving the purpose of throwing praseodymium.
Further, the saponification organic matter entering the above-mentioned dragout lanthanum extraction separation line is a saponification organic matter discharged from the dragout praseodymium extraction separation line, the dragout praseodymium extraction separation line is formed by the 1 st-40 st extraction tank section of the original neodymium samarium extraction separation line, the saponification organic matter is obtained after the blank organic matter is added with alkali for saponification, the saponification organic matter enters from the 1 st extraction tank of the dragout praseodymium extraction separation line, then gradually flows to the 40 th extraction tank of the dragout praseodymium extraction separation line, the dragout praseodymium extraction separation line is also divided into a rare earth soap section (1 st-20 th extraction tank) and an extraction section (21 st-40 st extraction tank), the praseodymium chloride solution discharged from the 1 st extraction tank of the dragout praseodymium extraction separation line enters from the 40 st extraction tank of the dragout praseodymium extraction separation line, flows to the 1 st extraction tank direction of the dragout praseodymium extraction separation line, is gradually mixed with the saponification organic matter in the dragout praseodymium extraction separation line, the 21 st extraction tank of the dragout praseodymium extraction separation line is subjected to multiple mixed extraction of the saponification organic matter, and the water phase discharged from 21 st extraction tank is the praseodymium chloride liquid, which can be used as the praseodymium chloride product. Correspondingly, in order to keep the water phase balance of the praseodymium extraction separation line, a part of praseodymium chloride feed liquid discharged from the 21 st extraction tank needs to reenter the praseodymium extraction separation line, namely, a part of praseodymium chloride feed liquid is taken as rare earth soap material, enters from the 20 th stage of the praseodymium extraction separation line and then flows out from the 1 st extraction tank, in the 1 st-20 th rare earth soap stage of the praseodymium extraction separation line, the saponified organic is continuously fished out of the praseodymium chloride feed liquid, then the praseodymium chloride is released in the extraction stage (21 st-40 th stage), the water phase discharged from the 1 st extraction tank of the rare earth soap stage is rare earth wastewater without rare earth (praseodymium neodymium), and can be directly processed in a wastewater treatment station, and the discharged organic phase is taken as saponified organic of the lanthanoid extraction separation line after the 20 th extraction stage is extracted.
The invention relates to an extraction method for improving the output of praseodymium and neodymium and controlling the praseodymium content in the praseodymium and neodymium, which is based on combining the existing neodymium and samarium extraction separation line, and aims to improve the processing capacity and control the praseodymium and neodymium proportion. Thus, the output of the original 72-level neodymium-samarium extraction separation line is improved from 2.3t/d REO (rare earth quantity) to more than 3t/d REO (rare earth quantity), the processing capacity is obviously improved, a praseodymium-neodymium chloride product with the praseodymium content of 23-27% can be obtained, neodymium oxide is not required to be additionally added to adjust the praseodymium-neodymium distribution, and meanwhile, a high-praseodymium product with the purity of more than 99.5% can be obtained, the problems that the processing capacity of the existing neodymium-samarium extraction separation line is small, and expensive neodymium oxide is required to be added to adjust the praseodymium-neodymium distribution 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 set forth:
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-dragging separation line, which is formed by 1-40 level extraction tanks of the original neodymium-samarium extraction separation line, the middle section is a praseodymium-dragging neodymium separation line, which is formed by 1-32 level extraction tanks of the original idle lanthanum-dragging separation line, the rear section is a samarium-dragging gadolinium separation line, which is formed by 41-72 level extraction tanks of the original neodymium-samarium extraction separation line, the rear section 41 level extraction tank is fed with neodymium-samarium feed liquid, the concentration of praseodymium and neodymium in the neodymium samarium feed liquid is 233.5g/L, the concentration of samarium and europium gadolinium is 233.88g/L, the feed flow is 13.4L/s, the feed flow of hydrochloric acid feed liquid with the feed concentration of 5.5mol/L in the 69 th-stage extraction tank is 2.18L/min, the 57 th-stage production samarium and europium chloride gadolinium feed liquid, the concentration of samarium and europium gadolinium is 233.88g/L, the concentration of praseodymium and neodymium is 233.5g/L, the 72 th-stage production blank organic matter is recycled, and the 72 th-stage water phase is returned forward. The 1/3 total amount of samarium europium chloride gadolinium liquid enters from a 56 th extraction tank, and flows back, the water phase produced at a 41 st extraction tank directly enters into a 32 nd extraction tank of a praseodymium and neodymium separation line, and the organic phase produced at the 32 nd extraction tank of the praseodymium and neodymium separation line directly enters into the 41 st extraction tank of the samarium europium and gadolinium separation line. Praseodymium and neodymium are separated from praseodymium and neodymium chloride produced in the 12 th stage of the line, and the praseodymium is distributed about 24w percent. And (3) feeding 1/3 of the total amount of praseodymium and neodymium chloride solution into the 11 th extraction tank, refluxing, directly feeding the water phase discharged from the 1 st extraction tank into the 40 th extraction tank of the praseodymium and neodymium scooping separation line, and feeding the organic phase discharged from the 40 th extraction tank of the praseodymium and neodymium scooping separation line into the 1 st extraction tank of the praseodymium and neodymium scooping separation line. The 1 st extraction tank of the praseodymium separating line is used for feeding saponification organic, the rare earth content in the rare earth wastewater discharged from the 1 st extraction tank is 0.005g/L, the rare earth loss rate is in a controllable range, the praseodymium chloride feed liquid discharged from the 21 st extraction tank has the praseodymium concentration of 235.29g/L, and the praseodymium chloride feed liquid is subjected to carbon precipitation and other treatments to obtain praseodymium oxide with the purity of 99.5%. 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 concentration of the neodymium samarium solution is 235.29g/L and the samarium europium gadolinium concentration is 233.88g/L. The production result is as follows: in the produced samarium europium chloride gadolinium 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 praseodymium is distributed by about 24 percent by weight; in the produced praseodymium chloride feed liquid, the concentration of praseodymium is 234.5g/L, and the purity of praseodymium oxide is 99.7%; 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 neodymium concentration of the neodymium samarium solution is 233.5g/L and the samarium europium gadolinium concentration is 233.88g/L. The production result is as follows: in the produced samarium europium chloride gadolinium 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 praseodymium is distributed by about 24 percent by weight; in the produced praseodymium chloride feed liquid, the concentration of praseodymium is 234.5g/L, and the purity of praseodymium oxide 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 was essentially the same as example 1 except that the original 72-stage samarium-neodymium extraction separation line was used, the process flow was as shown in fig. 2, and the other conditions were the same (e.g., the same concentration of samarium-neodymium feed solution was used). The production result is as follows: in the produced samarium europium chloride gadolinium 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 is about 28w percent, which is higher than the demand of the market praseodymium, and neodymium oxide is needed to be mixed to reduce the praseodymium; 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 foregoing description of the preferred embodiments of the invention is not intended to be limiting, but rather is intended to cover all modifications, equivalents, and alternatives falling within the spirit and principles of the invention.
Claims (9)
1. An extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in the praseodymium and neodymium is characterized by comprising the following steps:
A. setting a rare earth extraction separation line, wherein the rare earth extraction separation line comprises a praseodymium-dragging separation line, a praseodymium-dragging separation line and a samarium-europium-gadolinium separation line, the praseodymium-dragging separation line comprises a rare earth soap section and an extraction section, the praseodymium-dragging-europium-gadolinium separation line comprises a washing section and a back extraction section, and the praseodymium-dragging separation line, the praseodymium-dragging separation line and the samarium-europium-gadolinium separation line are all formed by serially connecting multiple extraction tanks;
B. the method comprises the steps of (1) carrying out treatment on a neodymium-samarium feed liquid and a saponified organic feeding and fishing samarium-europium-gadolinium separation line through a washing section and a back extraction section to obtain blank organic and samarium-europium-gadolinium chloride feed liquid in the back extraction section, and carrying out mixed extraction on part of samarium-europium-gadolinium chloride feed liquid after refluxing to a washing soap section to obtain praseodymium-neodymium chloride solution;
C. the praseodymium and neodymium chloride solution enters as a water phase of an extraction section of a separation line of the praseodymium and neodymium, and is treated by the extraction section to obtain praseodymium and neodymium chloride feed liquid with qualified praseodymium and neodymium distribution, and an organic phase discharged from the separation line of the praseodymium and neodymium is used as a saponification organic phase of the separation line of the samarium and europium; partially refluxing the obtained qualified praseodymium chloride neodymium feed liquid to a rare earth soap section for mixed extraction to obtain praseodymium chloride solution;
D. the method comprises the steps of taking praseodymium chloride solution as a water phase of an extraction section of a praseodymium scooping separation line, allowing saponified organic to flow in from the rare earth soap section of the praseodymium scooping separation line, allowing the saponified organic to flow out from the extraction section, processing the liquid by the extraction section to obtain praseodymium chloride feed liquid, taking the discharged organic phase as a saponified organic phase of the praseodymium scooping separation line, and allowing the obtained praseodymium chloride feed liquid to partially flow back to the rare earth soap section for mixed extraction to obtain rare earth wastewater.
2. The extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium according to claim 1, wherein the separation line of the praseodymium and neodymium comprises 30-60 extraction tanks, the separation line of the praseodymium and neodymium comprises 20-40 extraction tanks, and the separation line of the samarium and europium and gadolinium comprises 20-40 extraction tanks.
3. The extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium according to claim 2, wherein the separation line of the praseodymium and neodymium is composed of a rare earth soap section and an extraction section of a separation line of neodymium and samarium extraction, the separation line of the samarium and europium and gadolinium is composed of a washing section and a back extraction section of the separation line of the neodymium and samarium extraction, and the separation line of the praseodymium and neodymium is composed of a separation line of lanthanum and neodymium.
4. The extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium according to claim 3, wherein the extraction tanks connected in series with the neodymium-samarium extraction separation line are 72 stages in total, the first 40 stages of extraction tanks of the neodymium-samarium extraction separation line form a praseodymium-dragging separation line, the last 32 stages of the neodymium-samarium extraction separation line form a samarium-dragging europium-gadolinium separation line, and the extraction tanks connected in series with the lanthanum-dragging separation line are 32 stages in total.
5. The method for extracting praseodymium and neodymium from praseodymium and neodymium content control as claimed in claim 4, wherein the first 20 extraction tanks of the separation line of neodymium and samarium extraction are rare earth soap sections, the second 20 extraction tanks are extraction sections, the 41 st to 56 th extraction tanks of the separation line of neodymium and samarium extraction are washing sections, and the 57 th to 69 th extraction tanks are stripping sections; the first 11-stage extraction tank of the lanthanum fishing separation line is a rare earth soap section, and the second 21-stage extraction tank is an extraction section.
6. The extraction method of claim 5, wherein the capacity of the single extraction tank of the separation line of draging lanthanum is greater than the capacity of the single extraction tank of the separation line of neodymium samarium.
7. The method for extracting praseodymium and neodymium for increasing output and controlling praseodymium and neodymium content according to claim 6, wherein the neodymium liquid enters from a 41 st extraction tank of a neodymium-samarium extraction separation line, the hydrochloric acid solution enters from a 69 th extraction tank of the neodymium-samarium extraction separation line, the 57 th extraction tank of the neodymium-samarium extraction separation line discharges samarium europium chloride liquid, part of samarium europium chloride liquid flows back from a 56 th extraction tank to 41 st discharge praseodymium neodymium chloride solution; the praseodymium neodymium chloride solution enters from a 32 th extraction tank of a lanthanum fishing separation line, the praseodymium neodymium chloride solution is qualified and distributed from a 12 th extraction tank, part of the praseodymium neodymium chloride solution flows back from an 11 th extraction tank to a 1 st extraction tank, and the praseodymium chloride solution is discharged; the praseodymium chloride solution enters from a 40 th extraction tank of the praseodymium scooping separation line, the qualified praseodymium chloride feed liquid is discharged from a 21 st extraction tank, part of the praseodymium chloride feed liquid flows back from a 20 th extraction tank, the rare earth wastewater is discharged from a 1 st extraction tank of the praseodymium scooping separation line, and saponified organic enters from the 40 th extraction tank of the praseodymium scooping separation line.
8. The extraction method for improving the output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium according to claim 7, wherein the reflux amount of the samarium europium chloride gadolinium liquid is 1/4-2/3 of the total amount thereof; the reflux amount of praseodymium chloride neodymium feed liquid is 1/4-2/3 of the total amount of the praseodymium chloride neodymium feed liquid; the reflux amount of 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 output of praseodymium and neodymium and controlling the content of praseodymium in praseodymium and neodymium according to claim 1, wherein the feeding flow rate of the samarium liquid is 10-20L/s.
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