1. A calcium saponification organic phase clarification extraction process is characterized by comprising the following steps:

s1, preparing lime milk liquid by a plurality of lime milk preparation barrels, wherein the concentration of the lime milk liquid is 4.91-5.11 mol/L;

s2, washing of blank organic phase: fully stirring and mixing blank organic phase from a back extraction section of an extraction production line and raffinate waste water after separation of recovered rare earth soap waste water, and clarifying to obtain clear organic phase and washing waste water of the organic phase in the recovered rare earth soap waste water;

s3, calcium saponification: and (3) feeding the lime milk slurry obtained in the step (S1) and the blank organic phase obtained in the step (S2) into a calcium soap tank for multi-stage co-current continuous stirring and mixing to obtain a calcium saponified organic phase, wherein the volume flow ratio of the lime milk slurry to the blank organic phase is 0.108: 1, the saponification value of the calcium saponification organic phase is 0.44mol/L-0.64 mol/L;

s4, clarification: clarifying and filtering the calcium saponification organic phase in the S3 in a first organic clarifying pot to obtain a calcium saponification extracting agent, a water phase and insoluble particulate matters, feeding the clarified calcium saponification extracting agent into a transfer barrel, pumping the water phase to a wastewater treatment station after oil separation through a multi-stage oil separation tank, filter-pressing the insoluble particulate matters through a plate frame, merging the filtrate into the oil separation tank, and packaging the filter cake to be general solid waste;

s5, extraction: the calcium saponification extracting agent obtained from S4 and the rare earth soap material are mixed according to the volume flow ratio The method comprises the following steps of mixing, controlling the flow rate of a calcium saponification extracting agent and the rare earth soap stock, adding the mixture into a multistage co-current extraction stirring tank, mixing the calcium saponification extracting agent and the rare earth soap stock to form a mixture, carrying out a displacement reaction on the mixture, extracting rare earth ions, entering an organic phase, displacing calcium ions in the organic phase, entering the mixture into a second organic clarifying pot, and separating by the second organic phase clarifying pot to obtain a saturated organic phase containing the rare earth ions and a high-concentration calcium chloride aqueous solution.

S6, rare earth extraction and separation: the saturated organic phase obtained in S5 is pumped to the extraction line as required by the extraction process.

2. The lime saponification organic phase clarification extraction process of claim 1, wherein the pH value of the recovered rare earth soap waste water in step 2 is 4.0-5.0, and the pH value of the washing waste water is 1.0-3.0.

3. The calcium saponification organic phase clarification extraction process according to claim 1, wherein the chlorinated lime cream slurry in the step 5 is crystallized and separated out, and the residual water phase after the chlorinated lime cream slurry is crystallized and separated out is pumped to pass through a plate-frame filter press.

4. The calcium saponification organic phase clarification process of claim 1, wherein the multi-stage oil separation tank in step 4 is arranged between the first organic clarification pot and the extraction stirring tank and communicated with the first organic clarification pot, and the aqueous phase is divided into the multi-stage oil separation tank.

5. The lime saponification organic phase clarification extraction process of claim 1, wherein the lime saponification extracting agent obtained in step 4 is firstly fed into a transfer barrel, and then is added into the extraction stirring tank to be mixed with the rare earth soap stock, and the transfer barrel is communicated with the first organic clarification pot and the extraction stirring tank through a pipeline.

6. The lime saponification organic phase clarification extraction process of claim 1, wherein the rare earth soap stock in step 5 has a solubility of 10 g/ml.

7. The calcium saponification organic phase clarification extraction process of claim 1, wherein the temperature of the rare earth soap stock is controlled to be 36-65 ℃ in the whole process flow.

8. A calcium saponification organic phase clarification extraction device is applied to the extraction process according to any one of claims 1 to 7, and is characterized by comprising a reaction tank and a first stirring device, wherein the reaction tank is arranged in the previous process of the calcium soap tank and is communicated with the calcium soap tank, the first stirring device is positioned in the center of the first organic clarification pot and extends along the height direction of the first organic clarification pot, and a gap is reserved between the stirring device and the bottom of the first organic clarification pot.

9. The lime saponification organic phase refining extraction apparatus of claim 8, wherein a first phase separation weir is provided in the first organic refining kettle to separate the lime saponification extractant from the aqueous phase, the phase separation weir being adjustably positioned within the first organic refining kettle on one side of the agitation device to control the phase ratio of the lime saponification extractant to the aqueous phase.

10. The calcium saponification organic phase clarification extraction equipment according to claim 8, wherein a first adjusting pipe is further connected to the outside of the first organic clarification pot, and the first adjusting pipe is connected to the first stirring device, and the height of the first adjusting pipe is adjusted to control the phase ratio of the calcium saponification extracting agent and the water phase in the first organic clarification pot.

11. The calcium saponification organic phase clarification extraction equipment according to claim 8, further comprising a second organic clarification pot, wherein the second organic clarification pot is arranged in the next process of the extraction stirring tank, and the second organic clarification pot is communicated with the extraction stirring tank.

12. The lime saponification organic phase clarification extraction apparatus according to claim 11, wherein the second organic clarification pot comprises a second adjusting pipe, a second stirring device and a second phase separation weir plate, the second stirring device is located at the center of the second organic clarification pot, the second phase separation weir plate is located at one side of the second stirring device, and the second adjusting pipe is communicated with the lower end of the stirring device.

13. The lime saponification organic phase clarification extraction equipment according to claim 12, further comprising a transfer tank, wherein the transfer tank is arranged between the extraction stirring tank and the second organic clarification pot, and the transfer tank is respectively communicated with the extraction stirring tank and the second organic clarification pot.

Background

Because the iron slag discharged from the waste material also contains a small amount of rare earth, the invention aims to take out the rare earth in the iron slag through organic enrichment. Generally, an acidic extractant is adopted for extraction and separation of rare earth, the extraction process is carried out under a low acidity condition, generally, one rare earth ion is extracted to replace three H & lt + & gt to enter a water phase, the concentration of the H & lt + & gt in the water phase is continuously increased along with the continuous operation of the extraction process, the rare earth extraction capacity of the extractant is continuously reduced, and the extraction process cannot be stably carried out.

As is well known, the existing rare earth enrichment extraction process is to form rare earth carbonate particle precipitate by contacting rare earth with calcium carbonate, and then to add a certain amount of acid into the rare earth carbonate precipitate to dissolve the rare earth carbonate particle precipitate. The process of adding acid needs to be kept by people until the rare earth carbonate precipitate is dissolved to form the final feed liquid. The process is complex, and the manual operation has certain difficulty, so that aiming at the problems, the invention researches and develops the extraction process which is simple and can improve the operation difficulty of the staff.

Disclosure of Invention

In order to solve the above problems in the prior art, the present invention aims to provide a calcium saponification organic phase clarification extraction process, which aims to treat a large amount of three phases generated in the calcium saponification extraction process, and simplify the process flow of three-phase treatment operation to obtain a rare earth saturated organic phase.

In order to realize the purpose of the invention, the technical scheme adopted by the invention is as follows:

a calcium saponification organic phase clarification extraction process comprises the following steps:

s1, preparing lime milk liquid by a plurality of lime milk preparation barrels, wherein the concentration of the lime milk liquid is 4.91-5.11 mol/L;

s2, washing of blank organic phase: fully stirring and mixing blank organic phase from a back extraction section of an extraction production line and raffinate waste water after separation of recovered rare earth soap waste water, and clarifying to obtain clear organic phase and washing waste water of the organic phase in the recovered rare earth soap waste water;

s3, calcium saponification: and (3) feeding the lime milk slurry obtained in the step (S1) and the blank organic phase obtained in the step (S2) into a calcium soap tank for multi-stage co-current continuous stirring and mixing to obtain a calcium saponified organic phase, wherein the volume flow ratio of the lime milk slurry to the blank organic phase is 0.108: 1, the saponification value of the calcium saponification organic phase is 0.44mol/L-0.64 mol/L;

s4, clarification: clarifying and filtering the calcium saponification organic phase in the S3 in a first organic clarifying pot to obtain a calcium saponification extracting agent, a water phase and insoluble particulate matters, feeding the clarified calcium saponification extracting agent into a transfer barrel, pumping the water phase to a wastewater treatment station after oil separation through a multi-stage oil separation tank, filter-pressing the insoluble particulate matters through a plate frame, merging the filtrate into the oil separation tank, and packaging the filter cake to be general solid waste;

s5, extraction: and (3) mixing the calcium saponification extracting agent obtained from S4 and the rare earth soap material according to the volume flow ratio of 1:the method comprises the following steps of mixing, controlling the flow rate of a calcium saponification extracting agent and the rare earth soap stock, adding the mixture into a multistage co-current extraction stirring tank, mixing the calcium saponification extracting agent and the rare earth soap stock to form a mixture, carrying out a displacement reaction on the mixture, extracting rare earth ions, entering an organic phase, displacing calcium ions in the organic phase, entering the mixture into a second organic clarifying pot, and separating by the second organic phase clarifying pot to obtain a saturated organic phase containing the rare earth ions and a high-concentration calcium chloride aqueous solution.

S6, rare earth extraction and separation: the saturated organic phase obtained in S5 is pumped to the extraction line as required by the extraction process.

Optionally, the pH value of the recovered rare earth soap waste water in the step 2 is 4.0-5.0, and the pH value of the washing waste water is 1.0-3.0.

Optionally, the chloridized lime milk liquid crystal in the step 5 is formed into crystals and separated out, and the residual water phase after the chloridized lime milk liquid crystal is separated out is pumped into a plate frame for filter pressing.

Optionally, in step 4, the multistage oil separation tank is disposed between the first organic clarifying kettle and the extraction stirring tank and communicated with the first organic clarifying kettle, and the water phase is distributed to the multistage oil separation tank.

Optionally, the calcium saponification extracting agent obtained in step 4 needs to be fed into a transfer barrel, and then added into the extraction stirring tank to be mixed with the rare earth soap stock, wherein the transfer barrel is communicated with the first organic clarifying kettle and the extraction stirring tank through a pipeline.

Optionally, the rare earth soap stock in step 6 has a solubility of 10 g/ml.

Optionally, the temperature of the rare earth soap stock is controlled to be 36-65 ℃ in the whole process flow.

The invention also provides calcium saponification organic phase clarification extraction equipment which is applied to the calcium saponification organic phase clarification extraction process and comprises a reaction tank and a first stirring device, wherein the reaction tank is arranged in the previous working procedure of the calcium soap tank and is communicated with the calcium soap tank, the first stirring device is positioned in the center of the first organic clarification pot and extends along the height direction of the first organic clarification pot, and a gap is reserved between the stirring device and the bottom of the first organic clarification pot.

Optionally, a first phase separation weir is disposed in the first organic clarifier kettle to separate the calcium saponified extractant from the aqueous phase, and the phase separation weir is adjustably disposed inside the first organic clarifier kettle and on a side of the stirring device to control a phase ratio of the calcium saponified extractant to the aqueous phase.

Optionally, a first adjusting pipe is further connected to the outside of the first organic clarifying pan, the first adjusting pipe is connected to the first stirring device, and the height of the first adjusting pipe is adjusted to control the phase ratio of the calcium saponification extracting agent to the aqueous phase in the first organic clarifying pan.

Optionally, the calcium saponification organic phase clarification extraction equipment further comprises a second organic clarification pot, the second organic clarification pot is arranged in the next process of the extraction stirring tank, and the second organic clarification pot is communicated with the extraction stirring tank.

Optionally, the second organic clarifying kettle comprises a second adjusting pipe, a second stirring device and a second phase separation weir plate, the second stirring device is located at the center of the second organic clarifying kettle, the second phase separation weir plate is located at one side of the second stirring device, and the second adjusting pipe is communicated with the lower end of the stirring device.

Optionally, the calcium saponification organic phase clarification extraction equipment further comprises a transfer tank, the transfer tank is arranged between the extraction stirring tank and the second organic clarification pot, and the transfer tank is respectively communicated with the extraction stirring tank and the second organic clarification pot.

The technical scheme of the invention is that an organic phase (lime milk liquid) is prepared firstly, specifically, an alkaline solution containing calcium ions is selected for preparing the organic phase, a blank organic phase from a back extraction section of an extraction production line is separated from recovered rare earth soap waste water to obtain extracted waste water, the extracted waste water is fully stirred and mixed, and the organic phase washing waste water in a clear organic phase and the recovered rare earth soap waste water is obtained after clarification. Mixing the lime milk liquid and the blank organic phase according to the volume flow ratio of 0.108: 1, entering a calcium soap tank for multi-stage co-current continuous stirring and mixing to obtain a calcium saponified organic phase, wherein the saponification value of the calcium saponified organic phase is 0.44-0.64 mol/L, the solubility of the rare earth soap waste water is 1200mg/L, the COD of the rare earth soap waste water is reduced to about 700mg/L after the rare earth soap waste water and a blank organic phase are fully stirred, the solubility of the organic phase in water is reduced due to the fact that the acidity of the rare earth soap waste water is increased in the reaction, the saponified organic phase is added into an extraction stirring tank, and impurities in the organic phase are exchanged in the water phase and are removed. In order to ensure the extraction saturation of the organic phase and simultaneously ensure that impurities in the calcium saponified organic phase can be well exchanged, a plurality of extraction stirring tanks can be adopted for carrying out the extraction, it needs to be noted that the calcium saponified organic phase is clarified and filtered in a first organic clarifying pot to obtain a calcium saponified extractant, a water phase and insoluble particulate matters, the clarified calcium saponified extractant enters a transfer barrel, the water phase is pumped to a wastewater treatment station after oil separation through a multi-stage oil separation tank, the insoluble particulate matters are filter-pressed through a plate frame, the filtrate is merged into the oil separation tank, a filter cake is packed to be general solid waste, and the calcium saponified extractant and the rare earth soap material have the volume flow ratio ofThe calcium saponification extracting agent and the rare earth soap stock are mixed according to the proportion, the flow rates of the calcium saponification extracting agent and the rare earth soap stock are controlled, and the mixture is added into a multistage co-current extraction stirring tank, and the calcium saponification extracting agent and the rare earth soap stock are added into the multistage co-current extraction stirring tankAnd mixing a saponification extracting agent with the rare earth soap stock to form a mixture, carrying out a displacement reaction on the mixture, extracting rare earth ions, entering an organic phase, displacing calcium ions in the organic phase, entering the mixture into a second organic clarifying pot, and separating by the second organic phase clarifying pot to obtain a saturated organic phase containing the rare earth ions and a high-concentration calcium chloride aqueous solution. Because the concentration of calcium chloride is high (more than 100g/L), crystals are easy to be separated out to block a process pipeline, and the clarified and separated water phase and three phases are pumped into a filter plate frame for filter pressing. Namely, after the crystallization is separated from the chlorinated lime milk slurry, waste water still remains, if the flow rate of the saturated organic phase of the rare earth ions is 1L/min, the saponification value of the 1L organic phase is 0.54mol/L, 0.27mol of calcium ions can be extracted, the concentration of the rare earth soap stock is generally more than 0.55mol/L, namely the flow rate of the rare earth soap stock is 0.18/0.55X 0.9-0.2945L/min, and the concentration of the calcium ions in the waste water is 0.27X 111/0.2945-101.75 g/L.

The technical scheme of the invention has simple process and high extraction efficiency, greatly reduces energy consumption and improves production efficiency.

Drawings

In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the structures shown in the drawings without creative efforts.

FIG. 1 is a flow diagram of an extraction process according to one embodiment of the present invention;

fig. 2 is a schematic structural view of the first organic clarifier in fig. 1.

The reference numbers illustrate:

reference numerals	Name (R)	Reference numerals	Name (R)
				100	Extraction equipment	50	Oil separating groove
10	Preparation barrel	60	Transfer barrel
				20	Saponification tank	70	Transfer trough
30	First organic clarifying pot	80	Second organic clarifying pan
				31	First stirring device	81	Second stirring device
32	First phase-splitting weir plate	82	Second phase-splitting weir plate
				33	First adjusting pipe	83	Second regulating tube
40	Extraction stirring tank	90	Reaction tank

The implementation, functional features and advantages of the object of the present invention will be further explained with reference to the accompanying drawings.

Detailed Description

The present invention is further illustrated below with reference to specific examples.

As shown in fig. 1 and 2, this example provides a calcium saponification organic phase clarification extraction process, comprising the following steps:

s1, preparing lime milk liquid by a plurality of lime milk preparation barrels, wherein the concentration of the lime milk liquid is 4.91-5.11 mol/L;

s2, washing of blank organic phase: fully stirring and mixing blank organic phase from a back extraction section of an extraction production line and raffinate waste water after separation of recovered rare earth soap waste water, and clarifying to obtain clear organic phase and washing waste water of the organic phase in the recovered rare earth soap waste water;

s3, calcium saponification: and (3) feeding the lime milk slurry obtained in the step (S1) and the blank organic phase obtained in the step (S2) into a calcium soap tank for multi-stage co-current continuous stirring and mixing to obtain a calcium saponified organic phase, wherein the volume flow ratio of the lime milk slurry to the blank organic phase is 0.108: 1, the saponification value of the calcium saponification organic phase is 0.44mol/L-0.64 mol/L;

s4, clarification: clarifying and filtering the calcium saponification organic phase in the S3 in a first organic clarifying pot to obtain a calcium saponification extracting agent, a water phase and insoluble particulate matters, feeding the clarified calcium saponification extracting agent into a transfer barrel, pumping the water phase to a wastewater treatment station after oil separation through a multi-stage oil separation tank, filter-pressing the insoluble particulate matters through a plate frame, merging the filtrate into the oil separation tank, and packaging the filter cake to be general solid waste;

s5, extraction: the calcium saponification extracting agent obtained from S4 and the rare earth soap material are mixed according to the volume flow ratio The method comprises the following steps of mixing, controlling the flow rate of a calcium saponification extracting agent and the rare earth soap stock, adding the mixture into a multistage co-current extraction stirring tank, mixing the calcium saponification extracting agent and the rare earth soap stock to form a mixture, carrying out a displacement reaction on the mixture, extracting rare earth ions, entering an organic phase, displacing calcium ions in the organic phase, entering the mixture into a second organic clarifying pot, and separating by the second organic phase clarifying pot to obtain a saturated organic phase containing the rare earth ions and a high-concentration calcium chloride aqueous solution.

S6, rare earth extraction and separation: the saturated organic phase obtained in S5 is pumped to the extraction line as required by the extraction process.

In this embodiment, a plurality of calcium solution preparation barrels 10 are provided, the plurality of calcium solution preparation barrels 10 are arranged side by side and are communicated with each other, it is understood that the plurality of calcium solution preparation barrels 10 can filter the lime milk slurry step by step to improve the accuracy of the lime milk slurry, the plurality of preparation barrels 10 are connected with the saponification tank 20 through a pipeline, the saponification tank 20 can be provided in multiple stages, the multistage saponification tank 20 is respectively connected with the blank organic phase rotary barrel 60 and the first organic clarifying pan 30 through pipelines, the blank organic phase can be understood as an aqueous solution, the blank organic phase is added into the rare earth soap waste water (washing liquid), the initial solubility (chemical oxygen demand) of the washing liquid is 1200mg/L-1300mg/L, and after the blank organic phase reacts with the rare earth soap waste water, the solubility of the rare earth soap waste water is reduced to 600mg/L-700mg/L, because the solubility of the rare earth soap waste water is reduced, the acidity value, namely the pH value, of the rare earth soap waste water is reduced, namely, the acidity is enhanced. Before calcium saponification of lime milk liquid, oil removal treatment is carried out on saponification residual liquid, and then the saponification residual liquid is discharged into waste liquid, rare earth saponification blank organic phase reacts with the lime milk liquid to form a calcium saponification organic phase, meanwhile, the saponification value of the calcium saponification organic phase is 0.44-0.64 mol/L, the saponification value refers to the content of alkali in the calcium saponification organic phase, the content of the alkali shows the strength of dissolved acid during reaction with rare earth, the calcium saponification organic phase is added into a rare earth soap material (washing liquid) to obtain the rare earth saponification organic phase, and therefore rare earth chloride is obtained.

The technical scheme of the invention is that an organic phase (lime milk liquid) is prepared firstly, specifically, an alkaline solution containing calcium ions is selected for preparing the organic phase, a blank organic phase from a back extraction section of an extraction production line is separated from recovered rare earth soap waste water to obtain extracted waste water, the extracted waste water is fully stirred and mixed, and the organic phase washing waste water in a clear organic phase and the recovered rare earth soap waste water is obtained after clarification. Mixing the lime milk liquid and the blank organic phase according to the volume flow ratio of 0.108: 1, entering a calcium soap tank for multi-stage co-current continuous stirring and mixing to obtain a calcium saponified organic phase, wherein the saponification value of the calcium saponified organic phase is 0.44-0.64 mol/L, the solubility of the rare earth soap waste water is 1200mg/L, the COD of the rare earth soap waste water is reduced to about 700mg/L after the rare earth soap waste water and a blank organic phase are fully stirred, the solubility of the organic phase in water is reduced due to the fact that the acidity of the rare earth soap waste water is increased in the reaction, the saponified organic phase is added into an extraction stirring tank, and impurities in the organic phase are exchanged in the water phase and are removed. In order to ensure the extraction saturation of the organic phase and simultaneously ensure that impurities in the calcium saponified organic phase can be well exchanged, a plurality of extraction stirring tanks can be adopted for carrying out the extraction, it needs to be noted that the calcium saponified organic phase is clarified and filtered in a first organic clarifying pot to obtain a calcium saponified extractant, a water phase and insoluble particulate matters, the clarified calcium saponified extractant enters a transfer barrel, the water phase is pumped to a wastewater treatment station after oil separation through a multi-stage oil separation tank, the insoluble particulate matters are filter-pressed through a plate frame, the filtrate is merged into the oil separation tank, a filter cake is packed to be general solid waste, and the calcium saponified extractant and the rare earth soap material have the volume flow ratio ofThe method comprises the following steps of mixing, controlling the flow rate of a calcium saponification extracting agent and the rare earth soap stock, adding the mixture into a multistage co-current extraction stirring tank, mixing the calcium saponification extracting agent and the rare earth soap stock to form a mixture, carrying out a displacement reaction on the mixture, extracting rare earth ions, entering an organic phase, displacing calcium ions in the organic phase, entering the mixture into a second organic clarifying pot, and separating by the second organic phase clarifying pot to obtain a saturated organic phase containing the rare earth ions and a high-concentration calcium chloride aqueous solution. Because the concentration of calcium chloride is high (more than 100g/L), crystals are easy to be separated out to block a process pipeline, and the clarified and separated water phase and three phases are pumped into a filter plate frame for filter pressing. Namely, after the crystallization is separated from the chlorinated lime milk slurry, waste water still remains, if the flow rate of the saturated organic phase of the rare earth ions is 1L/min, the saponification value of the 1L organic phase is 0.54mol/L, 0.27mol of calcium ions can be extracted, the concentration of the rare earth soap stock is generally more than 0.55mol/L, namely the flow rate of the rare earth soap stock is 0.18/0.55X 0.9-0.2945L/min, and the concentration of the calcium ions in the waste water is 0.27X 111/0.2945-101.75 g/L.

In this embodiment, the PH of the recovered rare earth soap waste water in step 2 is 4.0 to 5.0, and the PH of the washing waste water is 1.0 to 3.0.

The pH value of the recovered rare earth soap waste water before reaction with a blank organic phase from a back extraction section of a production line is 4.0-5.0, the acid is weak, after the blank organic phase is added, the reaction is clarified to obtain a clear organic phase and washing waste water of the organic phase in the recovered rare earth soap waste water, and the pH value of the final washing waste water is 1.0-3.0, namely the solubility of the rare earth soap waste water is reduced, the acidity is enhanced, namely the pH value is reduced, and the reaction efficiency of the rare earth soap waste blank organic phase in the next process is improved.

In the embodiment, the chlorinated lime cream slurry in the step 5 is formed into crystals, and the residual aqueous phase after the chlorinated lime cream slurry crystals are separated out is pumped into a plate frame for filter pressing.

And 3, obtaining calcium saponification waste water after calcium saponification, and performing oil removal treatment on the calcium saponification waste water to improve the purity of the calcium saponification organic phase. In this embodiment, a multi-stage oil separating tank 50 is further included, the multi-stage oil separating tank 50 is disposed between the first organic clarifying pan 30 and the extraction stirring tank 40, and is communicated with the first organic clarifying pan 30, and the calcium saponification waste water is distributed into the multi-stage oil separating tank 50.

Deoiling is handled through setting up oil separating groove 50, and oil separating groove 50 is connected with first organic clarification pot 30 through organic looks pipe, specifically, oil separating groove 50 can set up multistage, and multistage oil separating groove 50 passes through pipeline interconnect, sets up multistage oil separating groove 50 and can help calcium saponification organic phase purification, improves the reaction efficiency of calcium saponification extractant and tombarthite washing water for reaction rate. After impurity removal, the content of U, Th in the hollow white organic phase in the tank body is below 10 percent, the extraction capacity of the organic phase is improved, and compared with the original untreated blank organic phase, the extraction capacity of the organic phase recycled after pretreatment is improved by more than 30 percent.

In this embodiment, the calcium saponification extracting agent obtained in step 4 needs to be first input into a transfer barrel 60, and then added into the extraction stirring tank 40 to be mixed with the rare earth soap stock, and the transfer barrel is communicated with the first organic clarifying kettle and the extraction stirring tank through a pipeline.

Understandably, the transfer barrel 60 is used for containing the calcium saponification extracting agent, the transfer barrel 60 is respectively connected with the extraction stirring tank 40 and the first organic clarifying pan 30 through pipelines, and the transfer barrel 60 is arranged to further precipitate the calcium saponification extracting agent, so that the reaction efficiency is improved.

In the embodiment, the solubility of the rare earth in the step 6 is 10g/ml, and the temperature of the rare earth soap stock is controlled to be 36-65 ℃ in the whole process flow.

The solubility of the rare earth before reaction is 10g/ml, namely the rare earth with low solubility, and the acid content in the rare earth with low solubility is less, so the extractant needs to be saponified before extraction and separation, and the alkali content of the extractant after saponification is higher, so that the extractant can conveniently react with a small amount of acid in the rare earth soap stock. In the whole process flow, the temperature of the sodium oxalate washing liquid is controlled to be 36-65 ℃ so as to prevent crystallization and ensure the washing efficiency.

The embodiment also provides a lime saponification organic phase clarification extraction equipment 100, is applied to above-mentioned lime saponification organic phase clarification extraction technology, including reaction tank 90 and first agitating unit 31, reaction tank 90 locates the former process in lime soap groove, and with lime soap groove intercommunication sets up, first agitating unit 31 is located the central point of first organic clarification pot 30 puts, and follows the direction of height extension setting of first organic clarification pot 30, just agitating unit with the clearance is left to the bottom of first organic clarification pot 30.

The reaction tank 90 is filled with rare earth soap waste water, the blank organic phase is added into the reaction tank 90 filled with the rare earth soap waste water, and the mixture is stirred to be fully reacted and mixed and then enters the saponification section for saponification. The bottom of the first organic clarifying pan 30 is provided with a discharge hole, the calcium saponification extracting agent is stirred by the first stirring device 31, so that the reaction of the internal solution is accelerated, and then the unreacted particles are completely sunk to the bottom of the first organic clarifying pan 30, so that the clarifying and filtering process of the extracting agent is realized. The first stirring device 31 is located at the center of the first organic refining pot 30, and the first stirring device 31 extends along the height direction of the first organic refining pot 30 and has a gap with the bottom of the first organic refining pot 30 to ensure that the first stirring device 31 can rotate inside the first organic refining pot 30. Specifically, first agitating unit 31 includes two blades, rotation axis and driving piece, the top of first organic clarification pot 30 is located to the driving piece, and the drive end of driving piece is connected to the one end of rotation axis, and the other end inserts the inside of first organic clarification pot 30 by the top of first organic clarification pot 30, and two blades set up on the rotation axis along the rotation direction interval of rotation axis, start the driving piece, and the driving piece drives the rotation axis rotation to drive the blade and rotate, in order to realize the stirring work of first agitating unit 31.

In this embodiment, as shown in fig. 2, a first phase separation weir 32 is disposed in the first organic clarifier kettle 30 to separate the lime-saponified extractant from the aqueous phase, and the phase separation weir is adjustably disposed inside the first organic clarifier kettle 30 and on one side of the stirring device to control the phase ratio of the lime-saponified extractant to the aqueous phase.

It can be understood that the first phase separation weir plate 32 is a plate-shaped structure, specifically, two side edges of the first phase separation weir plate 32 are respectively arranged in front and back, two plate surfaces of the first phase separation weir plate 32 respectively face the conveying direction of the process flow, and the first phase separation weir plate 32 is arranged to extend along the height direction of the first organic clarifying pan 30, that is, the first phase separation weir plate 32 is vertically arranged, so as to achieve the purpose of isolating the calcium saponification extracting agent from the water phase.

In this embodiment, a first adjusting pipe 33 is further connected to the outside of the first organic clarifying pan 30, the first adjusting pipe 33 is connected to the first stirring device 31, and the height of the first adjusting pipe 33 is adjusted to control the ratio of the calcium saponification extracting agent to the aqueous phase in the first organic clarifying pan 30.

The first adjusting pipe 33 controls the height of the first stirring device 31, and since the first stirring device 31 is connected to the first phase separation weir plate 32, the height of the first stirring device 31 can be controlled to control the first phase separation weir plate 32, thereby realizing the control and adjustment of the ratio of the calcium saponification extracting agent to the aqueous phase.

In this embodiment, the second organic clarifying pan 80 includes a second adjusting pipe 83, a second stirring device 81 and a second phase separation weir plate 82, the second stirring device 81 is located at the center of the second organic clarifying pan 80, the second phase separation weir plate 82 is located at one side of the second stirring device 81, and the second adjusting pipe 83 is communicated with the lower end of the stirring device. It is understood that the second organic clarifier pan 80 is similar in structure to the first organic clarifier pan 30 and will not be described in detail herein.

In this embodiment, the calcium saponification organic phase clarification extraction equipment 100 further includes a transfer tank 70, the transfer tank 70 is disposed between the extraction stirring tank 40 and the second organic clarification pot 80, and the transfer tank 70 is respectively communicated with the extraction stirring tank 40 and the second organic clarification pot 80.

Understandably, the transit tank 70 is used for containing the rare earth calcium saponification organic phase, the transit tank 70 is connected with the second organic clarifying pan 80 through a pipeline, and the transit tank 70 is arranged to further precipitate the saturated organic phase of rare earth ions, so that the reaction efficiency is improved.

The present invention is not limited to the above-described alternative embodiments, and various other forms of products can be obtained by anyone in light of the present invention. The above detailed description should not be taken as limiting the scope of the invention, which is defined in the claims, and which the description is intended to be interpreted accordingly.