CN113046580B - Scandium extraction pretreatment system and treatment method of scandium-containing solution - Google Patents
Scandium extraction pretreatment system and treatment method of scandium-containing solution Download PDFInfo
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Abstract
The invention provides a scandium extraction pretreatment system and a treatment method of a scandium-containing solution, wherein the scandium extraction pretreatment system comprises: the quenching and tempering part is provided with a first inlet, a second inlet and a quenching and tempering liquid outlet, wherein the first inlet is used for inputting scandium-containing solution, the second inlet is used for inputting concentrated sulfuric acid, and the quenching and tempering liquid outlet is used for outputting quenching and tempering liquid; the aging and settling part is provided with a first overflow port, a first liquid inlet and a first slag discharge port which are distributed from top to bottom, and the first liquid inlet is communicated with the tempering liquid outlet; the fixed bed is provided with a second liquid inlet, a second overflow port and a second slag discharge port which are distributed from top to bottom, and the second liquid inlet is communicated with the first overflow port; the first conveying pump, the first slag discharge port and the second slag discharge port are communicated with the first conveying pump. By adopting the scheme, the content of solid particles in the scandium-containing solution can be effectively reduced, the aging and sedimentation process is completed, a plurality of tanks are not needed, the equipment investment is low, and the production period of the product is shortened.
Description
Technical Field
The invention relates to the field of scandium extraction pretreatment, in particular to a scandium extraction pretreatment system and a treatment method of a scandium-containing solution.
Background
Scandium is distributed in the crust very dispersively and is a typical dilute metal element. Scandium can only be comprehensively recovered, enriched, separated and extracted from raw materials with complex compositions because of the very low content of scandium in the minerals. At present, scandium enriched in byproducts such as uranium thorium ore, laterite-nickel ore, bauxite, ilmenite, zircon placer ore and the like is a scandium resource with industrial significance in nature.
In the process flow of extracting scandium from laterite-nickel ore, the temperature of a scandium-containing solution entering an extraction procedure is higher and reaches 50-60 ℃, and the scandium-containing solution contains supersaturated calcium sulfate and a small amount of solid particles, if the scandium-containing solution directly enters an extraction system, a third phase of extraction can be formed, the extraction efficiency is reduced, the loss of an extracting agent is caused, and the normal operation of production is influenced. Therefore, the scandium-containing solution needs to be pretreated, aged and kept stand for a certain time to reduce the temperature of the solution to room temperature, reduce the content of solid particles in the solution, and simultaneously reduce calcium ions entering an extraction system as much as possible, thereby stabilizing the production process.
For the pretreatment scheme, the common practice in the industry is to adopt a flat-bottom groove for standing and aging, at least three groove bodies are needed during aging and are respectively used for liquid feeding, standing and aging and liquid discharging, the equipment investment is large, the occupied area is large, and the production period of the product is long.
Disclosure of Invention
The invention provides a scandium extraction pretreatment system and a treatment method of a scandium-containing solution, which are used for optimizing the treatment of the scandium-containing solution.
To achieve the above object, according to one aspect of the present invention, there is provided a scandium extraction pretreatment system including: the system comprises a tempering part and a control part, wherein the tempering part is provided with a first inlet, a second inlet and a tempering liquid outlet, the first inlet is used for inputting a scandium-containing solution, the second inlet is used for inputting concentrated sulfuric acid, and the tempering liquid outlet is used for outputting tempering liquid; the aging and settling part is provided with a first overflow port, a first liquid inlet and a first slag discharge port which are distributed from top to bottom, and the first liquid inlet is communicated with the tempering liquid outlet; the fixed bed is provided with a second liquid inlet, a second overflow port and a second slag discharge port which are distributed from top to bottom, and the second liquid inlet is communicated with the first overflow port; and the first slag discharge port and the second slag discharge port are communicated with the first conveying pump.
Further, the fixed bed still includes the backward flow mouth, the backward flow mouth is located the second overflow mouth with between the slag discharge opening of second, scandium extraction pretreatment systems still includes: the fixed bed is communicated with the aging and settling part through the overflow middle groove, the overflow middle groove is provided with a third inlet, a fourth inlet and a liquid outlet, the third inlet is communicated with the first overflow port, the liquid outlet is communicated with the second liquid inlet, and the fourth inlet is communicated with the reflux port.
Further, the scandium extraction pretreatment system further comprises: and the second conveying pump is arranged on a pipeline communicated with the liquid outlet and the second liquid inlet.
Further, the position of the overflow middle tank is lower than the return opening, and the scandium extraction pretreatment system further comprises: and the first valve is arranged on a pipeline for communicating the fourth inlet with the return port.
Further, the scandium extraction pretreatment system further comprises: a liquid level meter connected with the fixed bed to detect the liquid level in the fixed bed; the first turbidity meter is connected with the aging settling part; the control part, the level gauge, first turbidity appearance with first valve all with the control part electricity is connected.
Further, the scandium extraction pretreatment system further comprises: the temperature monitoring meter is arranged at a first overflow port of the aging settling part; the first turbidity meter is connected with the aging settling part; and the second turbidity meter is connected with the conditioning part.
Further, the scandium extraction pretreatment system further comprises: the first liquid inlet valve is connected with the first inlet; a second inlet valve connected to the second inlet; the control part, first feed liquor valve the second feed liquor valve the temperature monitor the first turbidity appearance with the second turbidity appearance all with the control part electricity is connected.
Further, quenching and tempering portion includes first cell body and agitating unit, first entry the second entry with quenching and tempering liquid outlet all is located on the first cell body, agitating unit is located in the first cell body.
Further, the aging and settling part comprises a second tank body, a liquid distribution pipe, a settling inclined plate and a slag discharge hopper, the liquid distribution pipe and the settling inclined plate are both arranged in a cavity of the second tank body, the liquid distribution pipe is positioned below the settling inclined plate, the slag discharge hopper is positioned below the second tank body, and the slag discharge hopper is communicated with the cavity of the second tank body; the first overflow port and the first liquid inlet are positioned on the second groove body, and the first slag discharge port is positioned at the lower part of the slag discharge hopper.
Further, the fixed bed includes barrel, cone, draft tube and clarification structure, wherein, clarification structure sets up in the barrel, the draft tube passes clarification structure, the cone is located the below of barrel, the cone with the barrel intercommunication, clarification structure includes a plurality of resin particles, the second inlet is located the upper portion of draft tube, the second overflow mouth is located the upper portion of barrel, the second row of cinder notch is located the lower part of cone.
Another embodiment of the present invention provides a method for treating a scandium-containing solution, including: inputting a scandium-containing solution and concentrated sulfuric acid into a quenching and tempering section to prepare a quenching and tempering liquid in the quenching and tempering section; inputting the conditioning liquid into an aging settling part for settling solid particles; and conveying the solution overflowing from the aging settling part into a fixed bed for filtering, and overflowing the filtered solution from the upper part of the aging settling part.
Further, the method for treating a scandium-containing solution further includes: detecting the turbidity of the solution in the tempering part and the turbidity of the solution in the aging settling part; and adjusting the speed of inputting scandium-containing solution and concentrated sulfuric acid into the tempering part according to the comparison between the solution turbidity in the tempering part and the solution turbidity in the aging and settling part.
Further, the method for treating a scandium-containing solution further includes: detecting a temperature of a solution within the aging settling section; and adjusting the retention time of the solution in the aging settling part according to the temperature of the solution in the aging settling part.
Further, the method for treating a scandium-containing solution further includes: detecting the liquid level of the solution in the fixed bed; and stopping inputting the solution into the fixed bed under the condition that the liquid level of the solution in the fixed bed reaches a preset value, and refluxing the solution in the fixed bed to an overflow middle tank.
Further, the method for treating a scandium-containing solution further includes: periodically discharging the slurry in the aging settling part and the bottom of the fixed bed; and performing solid-liquid separation on the discharged slurry, and returning the scandium-containing solution obtained after separation to the quenching and tempering section.
Further, the mixing mass ratio of the scandium-containing solution to the concentrated sulfuric acid in the quenching and tempering section is 1: 0.01-0.2, wherein the pH value of the tempering liquid is 0.1-2; the retention time of the solution in the aging settling part is 12-72 h, the solution is naturally cooled to 20-35 ℃, and the turbidity of the solution is reduced by 50-95% after settling; the turbidity range of the solution overflowing from the fixed bed is 10-100 ppm, and the concentration range of calcium sulfate in the solution is 0.01-0.1%.
By applying the technical scheme of the invention, the invention provides a scandium extraction pretreatment system, which comprises: the quenching and tempering part is provided with a first inlet, a second inlet and a quenching and tempering liquid outlet, wherein the first inlet is used for inputting scandium-containing solution, the second inlet is used for inputting concentrated sulfuric acid, and the quenching and tempering liquid outlet is used for outputting quenching and tempering liquid; the aging and settling part is provided with a first overflow port, a first liquid inlet and a first slag discharge port which are distributed from top to bottom, and the first liquid inlet is communicated with the tempering liquid outlet; the fixed bed is provided with a second liquid inlet, a second overflow port and a second slag discharge port which are distributed from top to bottom, and the second liquid inlet is communicated with the first overflow port; the first conveying pump, the first slag discharge port and the second slag discharge port are communicated with the first conveying pump. By adopting the scheme, calcium sulfate in the solution can be separated out to form solid particles by mixing the scandium-containing solution and concentrated sulfuric acid in the tempering part, then the solution can realize sedimentation and coarse filtration in the aging and sedimentation part, and then the solution enters the fixed bed to realize fine filtration. By adopting the scheme, the content of solid particles in the scandium-containing solution can be effectively reduced, the aging and sedimentation process is completed, a plurality of tanks are not needed, the equipment investment is low, and the production period of the product is shortened. By adopting the scheme, the solution can be automatically and continuously treated and matched with the subsequent extraction process.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this application, illustrate embodiments of the invention and, together with the description, serve to explain the invention and not to limit the invention. In the drawings:
fig. 1 shows a schematic structural diagram of a scandium extraction pretreatment system provided by an embodiment of the present invention;
fig. 2 shows a schematic view of the structure of the aging settling section in fig. 1;
fig. 3 shows a schematic structural view of the fixed bed in fig. 1.
Wherein the figures include the following reference numerals:
10. a tempering part; 11. a first tank body; 12. a stirring device; 20. an aging settling part; 21. a second tank body; 22. a liquid distribution pipe; 23. a sedimentation sloping plate; 24. a slag discharge hopper; 30. a fixed bed; 31. a barrel; 32. a conical body; 33. a draft tube; 34. a clarification structure; 41. a first delivery pump; 42. a second delivery pump; 43. a first valve; 50. and (4) overflowing the intermediate tank.
Detailed Description
The technical solution in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 to 3, an embodiment of the present invention provides a scandium extraction pretreatment system, including: the quenching and tempering part 10 is provided with a first inlet, a second inlet and a quenching and tempering liquid outlet, wherein the first inlet is used for inputting scandium-containing solution, the second inlet is used for inputting concentrated sulfuric acid, and the quenching and tempering liquid outlet is used for outputting quenching and tempering liquid; the aging and settling part 20 is provided with a first overflow port, a first liquid inlet and a first slag discharge port which are distributed from top to bottom, and the first liquid inlet is communicated with the tempering liquid outlet; the fixed bed 30 is provided with a second liquid inlet, a second overflow port and a second slag discharge port which are distributed from top to bottom, and the second liquid inlet is communicated with the first overflow port; the first conveying pump 41, the first slag discharge port and the second slag discharge port are communicated with the first conveying pump 41.
By adopting the scheme, calcium sulfate in the solution can be separated out into solid particles by mixing the scandium-containing solution and concentrated sulfuric acid in the quenching and tempering part 10, then the solution can realize sedimentation and coarse filtration in the aging and sedimentation part 20, and then the solution enters the fixed bed 30 to realize fine filtration. By adopting the scheme, the content of solid particles in the scandium-containing solution can be effectively reduced, the aging and sedimentation process is completed, a plurality of tanks are not needed, the equipment investment is low, and the production period of the product is shortened.
In this embodiment, the fixed bed 30 further includes a return opening, the return opening is located between the second overflow opening and the second slag discharge opening, and the scandium extraction pretreatment system further includes: and the overflow middle groove 50, the fixed bed 30 is communicated with the aging settling part 20 through the overflow middle groove 50, the overflow middle groove 50 is provided with a third inlet, a fourth inlet and a liquid outlet, wherein the third inlet is communicated with the first overflow port, the liquid outlet is communicated with the second liquid inlet, and the fourth inlet is communicated with the return port. After the fixed bed 30 is used for a period of time, it will reach a saturated state, affecting the filtering effect. At this time, the solution in the fixed bed 30 may be refluxed to the overflow middle tank 50, and then the fixed bed 30 may be cleaned, thereby ensuring normal production. Therefore, the above arrangement can facilitate the cleaning of the fixed bed 30.
In this embodiment, the scandium extraction pretreatment system further includes: and a second delivery pump 42 disposed on a pipeline communicating the liquid outlet and the second liquid inlet. The second transfer pump 42 is used to transfer the solution in the overflow intermediate tank 50 to the fixed bed 30.
In this embodiment, the position of the overflow middle tank 50 is lower than the reflux port, and the scandium extraction pretreatment system further includes: and a first valve 43 provided in a line connecting the fourth inlet and the return port. The position of the overflow intermediate tank 50 below the reflux port facilitates the reflux of the solution in the fixed bed 30. During normal production, the first valve 43 is closed to prevent the solution in the fixed bed 30 from flowing back.
In this embodiment, the scandium extraction pretreatment system further includes a third pump body, and the third pump body is arranged on the pipeline that communicates quenching and tempering liquid export and first inlet. The third pump body is used for inputting the solution in the conditioning part 10 into the aging settling part 20.
In this embodiment, the scandium extraction pretreatment system further includes: a level meter connected to the fixed bed 30 to detect a liquid level in the fixed bed 30; a first turbidity meter connected with the aging settling part 20; the control part, the liquid level meter, the first turbidity meter and the first valve 43 are all electrically connected with the control part. The liquid level in the fixed bed 30 can be detected by a liquid level meter, and the turbidity of the solution in the upper part in the aging settling section 20 can be detected by a first turbidity meter. This allows the effectiveness of the fixed bed 30 to be determined, and if a significant increase in liquid level or a significant increase in turbidity is detected, the fixed bed 30 needs to be cleaned. Through the cooperation of control portion and different parts, can realize automated inspection and washing, improved degree of automation.
In this embodiment, the scandium extraction pretreatment system further includes: a temperature monitor disposed at a first overflow port of the aging settling part 20; a first turbidity meter connected with the aging settling part 20; the second turbidity meter is connected to the tempering unit 10. This allows the temperature and turbidity of the solution in the aged-precipitation portion 20 to be detected on-line, and the turbidity of the solution in the quenched and tempered portion 10 to be detected. The production conditions can be adjusted by the detected values to improve the sedimentation effect.
In this embodiment, the scandium extraction pretreatment system further includes: the first liquid inlet valve is connected with the first inlet; the second liquid inlet valve is connected with the second inlet; the control part, first feed liquor valve, second feed liquor valve, temperature monitor, first turbidity appearance and second turbidity appearance all are connected with the control part electricity. Through the arrangement, parameters such as the injection amount and the injection speed of the scandium-containing solution and the concentrated sulfuric acid can be adjusted according to the detection result, so that the production process is optimized.
In this embodiment, the tempering part 10 includes a first tank 11 and a stirring device 12, the first inlet, the second inlet and the outlet of the tempering liquid are all located on the first tank 11, and the stirring device 12 is located in the first tank 11. The mixed solution can be stirred by the stirring device 12 so that the solution is mixed sufficiently.
In this embodiment, the aging settling part 20 includes a second tank 21, a liquid distribution pipe 22, a settling sloping plate 23 and a slag discharge hopper 24, the liquid distribution pipe 22 and the settling sloping plate 23 are both disposed in a cavity of the second tank 21, the liquid distribution pipe 22 is located below the settling sloping plate 23, the slag discharge hopper 24 is located below the second tank 21, and the slag discharge hopper 24 is communicated with the cavity of the second tank 21; the first overflow port and the first liquid inlet are positioned on the second groove body 21, and the first slag discharge port is positioned at the lower part of the slag discharge hopper 24. Through the arrangement, the settling effect of solid particles in the solution can be improved. The solution with less solid particles overflows from the upper part of the second groove body 21 to continue the treatment.
Specifically, the fixed bed 30 comprises a cylinder 31, a cone 32, a guide cylinder 33 and a clarification structure 34, wherein the clarification structure 34 is arranged in the cylinder 31, the guide cylinder 33 passes through the clarification structure 34, the cone 32 is positioned below the cylinder 31, the cone 32 is communicated with the cylinder 31, the clarification structure 34 comprises a plurality of resin particles, a second liquid inlet is positioned at the upper part of the guide cylinder 33, a second overflow port is positioned at the upper part of the cylinder 31, and a second slag discharge port is positioned at the lower part of the cone 32. The solution entering from the guide cylinder 33 is filtered by the clarifying structure 34 and then overflows from the upper part of the cylinder 31, thus improving the filtering effect.
Another embodiment of the present invention provides a method for treating a scandium-containing solution, including: a scandium-containing solution and concentrated sulfuric acid are fed into the quenching and tempering section 10 to prepare a quenching and tempering solution in the quenching and tempering section 10; feeding the conditioned liquid into an aging settling section 20 to settle solid particles; the solution overflowing from the aging settling section 20 is introduced into the fixed bed 30 and filtered, and the filtered solution overflows from the upper part of the aging settling section 20.
Further, the method for treating the scandium-containing solution further includes: detecting the turbidity of the solution in the tempering part 10 and the solution in the aging settling part 20; the speed of feeding the scandium-containing solution and the concentrated sulfuric acid into the conditioned section 10 is adjusted according to the comparison between the turbidity of the solution in the conditioned section 10 and the turbidity of the solution in the aging settling section 20. Therefore, automatic detection and adjustment can be realized, and the production effect is ensured.
In this embodiment, the method for treating a scandium-containing solution further includes: detecting the temperature of the solution in the aging settling section 20; the residence time of the solution in aging settling section 20 is adjusted according to the solution temperature in aging settling section 20. This allows the solution in aging settling section 20 to be adjusted to a suitable temperature.
In this embodiment, the method for treating a scandium-containing solution further includes: detecting the level of the solution within the fixed bed 30; when the liquid level of the solution in the fixed bed 30 reaches a preset value, the supply of the solution into the fixed bed 30 is stopped, and the solution in the fixed bed 30 is returned to the overflow intermediate tank 50. Whether the fixed bed 30 normally works can be judged through the liquid level height, if the liquid level is too high, solid particles in the fixed bed 30 are saturated, the solution flowing is blocked, and at the moment, the solution in the fixed bed 30 flows back to the overflow middle tank 50, so that the fixed bed 30 is convenient to clean. The method realizes automatic and continuous production.
In this embodiment, the method for treating a scandium-containing solution further includes: periodically discharging the slurry at the bottom of the aging settling section 20 and the fixed bed 30; the discharged slurry is subjected to solid-liquid separation, and the scandium-containing solution obtained after the separation is returned to the quenching and tempering section 10. The scandium-containing solution obtained after the separation is returned to the quenching and tempering section 10, so that resource waste can be avoided.
Specifically, the mixing mass ratio of the scandium-containing solution to the concentrated sulfuric acid in the quenching and tempering section 10 is 1: 0.01-0.2, wherein the pH value of the tempering liquid is 0.1-2; the retention time of the solution in the aging settling part 20 is 12-72 h, the solution is naturally cooled to 20-35 ℃, and the turbidity of the solution is reduced by 50-95% after settling; the turbidity range of the solution overflowing from the fixed bed 30 is 10-100 ppm, and the concentration range of calcium sulfate in the solution is 0.01% -0.1%. By setting the above parameters, a good treatment effect of the scandium-containing solution can be ensured.
To facilitate understanding of the present solution, the following is further described.
In the prior art, a common method in the industry for a scandium-containing solution pretreatment scheme is to adopt a flat-bottom tank for standing and aging, and then pump the scandium-containing solution to a PE microporous filter tube fine filter for fine filtration. This solution has the following problems: 1. at least 3 groove bodies are needed for liquid feeding, standing and aging and liquid discharging during aging, so that the equipment investment is large, the occupied area is large, the product period is prolonged, and the occupation amount of the mobile capital of enterprises is increased; 2. the sedimentation particle layer at the bottom of the aging tank can generate disturbance when the aging tank discharges liquid, so that the sedimentation effect is poor; 3. the aging tank needs manual slag removal at regular intervals, and the labor intensity is high; 4. the micropore fine filter adopts PE micropore filter pipe to filter, and this filter pipe is the consumptive material, uses the unable regeneration of back because of the filter cake blocks up the micropore after a period, needs to change, increases the running cost.
The scheme mainly aims at the defects of the pretreatment process and provides a system and a method for pretreating scandium-containing solution.
The scandium-containing solution pretreatment system (i.e., scandium extraction pretreatment system) includes a quenching and tempering section, an aging and settling section, and a fixed bed. Wherein the tempering part comprises a tempering groove; the aging and settling part comprises a tempering solution pump and an aging and settling tank; the fixed bed comprises an overflow middle tank, an overflow pump, a fixed bed clarifier and a underflow pump.
The quenching and tempering tank is provided with a scandium-containing solution inlet, a concentrated sulfuric acid inlet and a quenching and tempering liquid outlet, the scandium-containing solution inlet and the concentrated sulfuric acid inlet are positioned at the top of the quenching and tempering tank, the quenching and tempering liquid outlet is positioned at the bottom of the side surface of the quenching and tempering tank, and 1 double-layer stirring paddle is arranged in the quenching and tempering tank. The aging settling tank is of a rectangular structure, the bottom of the aging settling tank is provided with a slag discharge hopper, the slag discharge hopper is provided with a tempering liquid inlet, an overflow outlet and a slag discharge port, the tempering liquid inlet is positioned at the bottom of the side face, the overflow outlet is positioned at the top of the side part opposite to the tempering liquid inlet, and the slag discharge port is positioned at the bottom of the slag discharge hopper. The overflow middle groove is provided with an overflow inlet, a backwashing liquid receiving port and an overflow discharging port, the overflow inlet and the backwashing liquid receiving port are positioned at the top of the groove, and the overflow liquid discharging port is positioned at the bottom of the side surface of the overflow middle groove. The slag discharging hopper is arranged at the bottom of the fixed bed clarifier, the groove body is provided with a liquid inlet, an overflow port, a backflow port and a slag discharging port, the liquid inlet is positioned at the top of the fixed bed clarifier, the overflow port is positioned at the top of the side wall, the backflow port is positioned at the bottom of the side wall, and the slag discharging port is positioned at the bottom of the slag discharging hopper.
Optionally, the scandium-containing solution is connected to a scandium-containing solution inlet of the tempering tank via a metering device. The concentrated sulfuric acid is connected with the concentrated sulfuric acid inlet of the quenching and tempering tank through the metering device, so that the input amount and the proportion of the solution can be conveniently monitored and controlled. And a conditioning liquid outlet of the conditioning tank is connected with a conditioning liquid inlet of the aging settling tank through a variable frequency centrifugal pump. The overflow outlet of the aging and tempering tank is connected with the overflow inlet of the overflow middle tank. The overflow discharge port of the overflow middle groove is connected with the liquid inlet of the fixed bed clarifier through a variable frequency centrifugal pump. The filtrate in the overflow middle groove is connected with the reflux port of the fixed bed clarifier.
Optionally, the tempering tank is of a cylindrical structure, and the double-layer paddle type stirring paddles of the stirring device are arranged on the stirring shaft in an upper layer and a lower layer and used for mixing the solution. The slag discharge port of the aging settling tank and the slag discharge port of the fixed bed clarifier are connected with a slag slurry pump. A plurality of liquid distribution pipes are arranged in the aging settling tank at the same height position as the tempering liquid inlet, and an overflow weir is arranged at the same height position as the overflow port. Optionally, a row of inclined plates (i.e. settling inclined plates) with an inclination angle of 45 ° are placed in the settling tank, and the distance between the inclined plates is about 80-100 mm.
Furthermore, the upper part of the fixed bed clarifier is cylindrical, and the lower part of the fixed bed clarifier is an inverted cone container. The center of the upper part of the clarifier is provided with a guide shell in the vertical direction. Optionally, a layer of steel wire mesh is arranged at the bottom and the outside of the guide shell along the radial direction, a layer of steel wire mesh is arranged at the joint of the conical shape and the inner cylinder of the container along the radial direction, and a plurality of resin particles with the diameter of about 3mm are filled in the clarifier. Thus, a good filtering effect can be achieved.
The invention also provides a method for the continuous treatment of a scandium-containing extraction solution (i.e. a method for the treatment of a scandium-containing solution), the method comprising the steps of:
the method comprises the following steps: the scandium-containing solution is sent into a tempering tank and mixed with concentrated sulfuric acid according to a certain proportion to prepare tempering liquid, and supersaturated calcium sulfate in the solution is separated out to form solid particles under the same ion effect of sulfuric acid;
step two: and (2) delivering the conditioning liquid in the step one into an aging settling tank by a pump, uniformly feeding the conditioning liquid into the aging settling tank under the action of a liquid distribution pipe, naturally settling larger solid particles into a slag discharge hopper, allowing fine solid particles to move upwards along with the flow direction of the solution, allowing the solid particles to be in contact with an inclined plate and settled down in a settling area formed by the inclined plate due to the change of the flow direction of the fluid, and also feeding the solution into the slag discharge hopper, wherein the solution enters an overflow port from an overflow weir at the upper part of the aging settling tank and is discharged. And a thermometer is arranged at the overflow outlet, and simultaneously the quenching and tempering liquid and the overflow turbidity are measured by an online turbidity meter and fed back to the control system. And the control system judges the sedimentation effect according to the comparison of the turbidity of the tempering liquid and the overflow, and the sedimentation effect is used as a basis for adjusting the current frequency of the liquid inlet pump.
Step three: and in the second step, the overflow is sent into a fixed bed clarifier through an overflow middle tank by using a variable frequency centrifugal pump. The clear water enters the bottom of the clarifier through the guide shell, passes through a fixed bed filtering area consisting of resin particles, is adsorbed by the resin particle balls, rises, is discharged through an overflow water pipeline, and finishes the fine filtering process. The turbidity of the overflow water is measured by an online turbidity meter and fed back to the control system. After a period of time, the resin particle ball of the filtering system can reach a saturated state, a rising water path is blocked, the liquid level of the guide cylinder rises, and the liquid level is fed back to the control system through the liquid level measurement of the ultrasonic liquid level meter. The control system judges through signal data fed back from the turbidity meter and the liquid level meter, and when the resin particle balls need to be backflushed, the control system controls the feed pump to be closed and the electric valve of the backflushing water pipe to be opened, so that the slurry in the fixed bed clarifier flows back into the overflow intermediate tank quickly. In the process of liquid level descending, friction is generated between resin particle balls due to disturbance, and adsorbed solid particles can settle and enter a slag discharge hopper, so that the aim of cleaning is fulfilled. After the cleaning process is finished (the ultrasonic liquid level meter provides a liquid level signal for judgment), the control system closes the electric valve of the backwashing water pipe, restarts the variable-frequency centrifugal pump for feeding liquid and carries out fine filtration.
Step four: and (4) opening the underflow pump periodically, discharging relatively high-concentration slurry at the bottoms of the aging settling tank and the fixed bed clarifier, and after carrying out liquid-solid separation, returning filtrate serving as scandium-containing solution to the quenching and tempering tank.
In the first step, the mixing mass ratio of the scandium-containing solution to the concentrated sulfuric acid is 1: 0.01-0.2, and the pH value of the conditioning liquid is controlled within the range of 0.1-2. Further, certain solutions without calcium sulfate can be directly subjected to the next step without tempering.
And in the second step, the retention time of the quenching and tempering liquid in the aging settling tank is 12-72 hours, the solution temperature is reduced to 20-35 ℃ after natural cooling, and the solution turbidity is reduced by 50-95% after passing through the aging settling tank.
The turbidity control range of the overflow in the third step is 10-100 ppm, and the concentration of calcium sulfate in the solution is less than 0.01-0.1%.
The illustrative embodiment using the above scheme is as follows:
example 1
(1) Feeding the scandium-containing solution at 60 ℃ into a tempering tank, and mixing the scandium-containing solution with concentrated sulfuric acid according to the proportion of 1:0.01 to prepare tempering liquid, wherein the pH value of the tempering liquid is 2;
(2) pumping the conditioning liquid obtained in the step (1) into an aging settling tank, adjusting the current frequency of a centrifugal pump for conveying the conditioning liquid, controlling the retention time of the solution in the tank to be 12h, and displaying by an online turbidity meter that the turbidity of the inlet liquid is 200ppm, the turbidity of an overflow outlet is 100ppm, the turbidity of the solution is reduced by 50%, and the overflow temperature is reduced to 35 ℃;
(3) conveying the overflow obtained in the step (2) into a fixed bed clarifier through an overflow intermediate tank by using a variable frequency centrifugal pump, and after fine filtration by the clarifier, wherein the turbidity in the overflow is 80ppm, and the concentration of calcium sulfate in the solution is 0.1%;
the removal rate of the solution calcium sulfate in the example is 60%, the turbidity is reduced to 80ppm, and the temperature is reduced to 35 ℃.
Example 2
(1) Feeding the scandium-containing solution at 50 ℃ into a tempering tank, and mixing the scandium-containing solution with concentrated sulfuric acid according to the proportion of 1:0.1 to prepare tempering liquid, wherein the pH value of the tempering liquid is 0.5;
(2) pumping the conditioning liquid obtained in the step (1) into an aging settling tank, adjusting the current frequency of a centrifugal pump for conveying the conditioning liquid, controlling the retention time of the solution in the tank to be 72 hours, and displaying by an online turbidity meter that the turbidity of the inlet liquid is 300ppm, the turbidity of an overflow outlet is 90ppm, the turbidity of the solution is reduced by 70%, and the overflow temperature is reduced to 25 ℃;
(3) conveying the overflow obtained in the step (2) into a fixed bed clarifier through an overflow intermediate tank by using a variable frequency centrifugal pump, and after fine filtration by the clarifier, wherein the turbidity in the overflow is 10ppm, and the concentration of calcium sulfate in the solution is 0.02%;
the removal rate of the solution calcium sulfate in this example was 90% and the turbidity was reduced to 10 ppm.
Example 3
(1) Feeding the scandium-containing solution at 55 ℃ into a tempering tank, and mixing the scandium-containing solution with concentrated sulfuric acid according to the proportion of 1:0.05 to prepare tempering liquid, wherein the pH value of the tempering liquid is 1.2;
(2) pumping the conditioning liquid obtained in the step (1) into an aging settling tank, adjusting the current frequency of a centrifugal pump for conveying the conditioning liquid, controlling the retention time of the solution in the tank to be 36h, and displaying by an online turbidity meter that the turbidity of the inlet liquid is 250ppm, the turbidity of an overflow outlet is 120ppm, the turbidity of the solution is reduced by 52 percent, and the overflow temperature is reduced to 30 ℃;
(3) conveying the overflow obtained in the step (2) into a fixed bed clarifier through an overflow intermediate tank by using a variable frequency centrifugal pump, and after fine filtration by the clarifier, wherein the turbidity in the overflow is 50ppm, and the concentration of calcium sulfate in the solution is 0.05%;
the removal rate of the solution calcium sulfate in this example was 70% and the turbidity was reduced to 50 ppm.
Example 5
(1) Feeding the scandium-containing solution at 55 ℃ into a tempering tank, and mixing the scandium-containing solution with concentrated sulfuric acid according to the proportion of 1:0.07 to prepare tempering liquid, wherein the pH value of the tempering liquid is 0.8;
(2) pumping the conditioning liquid obtained in the step (1) into an aging settling tank, adjusting the current frequency of a centrifugal pump for conveying the conditioning liquid, controlling the retention time of the solution in the tank to be 48 hours, and displaying by an online turbidity meter that the turbidity of the inlet liquid is 250ppm, the turbidity of an overflow outlet is 100ppm, the turbidity of the solution is reduced by 60 percent, and the overflow temperature is reduced to 28 ℃;
(3) conveying the overflow obtained in the step (2) into a fixed bed clarifier through an overflow intermediate tank by using a variable frequency centrifugal pump, and after fine filtration by the clarifier, wherein the turbidity in the overflow is 20ppm, and the concentration of calcium sulfate in the solution is 0.03%;
the removal rate of the solution calcium sulfate in this example was 80% and the turbidity was reduced to 20 ppm.
From the above, the scheme has the following characteristics or effects:
(1) the content of solid particles in the scandium-containing solution is effectively reduced, the aging and sedimentation process is completed, the equipment investment is low, and the production period is shortened;
(2) the aging settling tank discharges liquid through overflow, so that disturbance to settling underflow is reduced, and stable and continuous operation can be realized;
(3) the sediment bottom flow is discharged by pumping at regular intervals through the slag discharge hopper, so that the labor intensity is reduced;
(4) the device has long service life, the whole process has no consumable material, and the production and operation cost is saved;
(5) the device is automatically controlled by a control system, an automatic instrument, an automatic valve and a motor, and the whole process does not need manual intervention.
The above is only a preferred embodiment of the present invention, and is not intended to limit the present invention, and various modifications and changes will occur to those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (15)
1. A scandium extraction pretreatment system, comprising:
the quenching and tempering part (10) is provided with a first inlet, a second inlet and a quenching and tempering liquid outlet, wherein the first inlet is used for inputting a scandium-containing solution, the second inlet is used for inputting concentrated sulfuric acid, and the quenching and tempering liquid outlet is used for outputting the quenching and tempering liquid;
the aging and settling part (20), the aging and settling part (20) is provided with a first overflow port, a first liquid inlet and a first slag discharge port which are distributed from top to bottom, and the first liquid inlet is communicated with the tempering liquid outlet;
the fixed bed (30) is provided with a second liquid inlet, a second overflow port and a second slag discharge port which are distributed from top to bottom, and the second liquid inlet is communicated with the first overflow port;
the first conveying pump (41), the first slag discharge port and the second slag discharge port are communicated with the first conveying pump (41);
fixed bed (30) still includes the backward flow mouth, the backward flow mouth is located the second overflow mouth with between the second slag discharge port, scandium extraction pretreatment system still includes overflow intermediate trough (50), fixed bed (30) pass through overflow intermediate trough (50) with ageing settling portion (20) intercommunication, overflow intermediate trough (50) have third entry, fourth entry and liquid outlet, wherein, the third entry with first overflow mouth intercommunication, the liquid outlet with the second inlet intercommunication, the fourth entry with the backward flow mouth intercommunication.
2. The scandium extraction pretreatment system of claim 1, further comprising:
and the second conveying pump (42) is arranged on a pipeline communicated with the liquid outlet and the second liquid inlet.
3. Scandium extraction pretreatment system according to claim 1, characterized in that the overflow intermediate tank (50) is located below the return opening, the scandium extraction pretreatment system further comprising:
and a first valve (43) provided on a line connecting the fourth inlet and the return port.
4. The scandium extraction pretreatment system of claim 3, further comprising:
a liquid level meter connected to the fixed bed (30) to detect a liquid level within the fixed bed (30);
a first turbidity meter connected to the aging settling part (20);
the control part, level gauge, first turbidity appearance and first valve (43) all with the control part electricity is connected.
5. The scandium extraction pretreatment system of claim 1, further comprising:
a temperature monitor arranged at a first overflow port of the aging settling part (20);
a first turbidity meter connected to the aging settling part (20);
and a second turbidity meter connected to the conditioning unit (10).
6. The scandium extraction pretreatment system of claim 5, further comprising:
a first inlet valve connected to the first inlet;
a second inlet valve connected to the second inlet;
the first liquid inlet valve, the second liquid inlet valve, the temperature monitor, the first turbidity meter and the second turbidity meter are all electrically connected with the control part.
7. The scandium extraction pretreatment system according to claim 1, wherein the tempering section (10) comprises a first tank (11) and an agitation device (12), the first inlet, the second inlet and the outlet of the tempered liquid are all located on the first tank (11), and the agitation device (12) is located inside the first tank (11).
8. The scandium extraction pretreatment system according to claim 1, wherein the aging and settling section (20) comprises a second tank (21), a liquid distribution pipe (22), a settling inclined plate (23) and a slag discharge hopper (24), the liquid distribution pipe (22) and the settling inclined plate (23) are both arranged in a cavity of the second tank (21), the liquid distribution pipe (22) is located below the settling inclined plate (23), the slag discharge hopper (24) is located below the second tank (21), and the slag discharge hopper (24) is communicated with the cavity of the second tank (21); the first overflow port and the first liquid inlet are positioned on the second groove body (21), and the first slag discharge port is positioned at the lower part of the slag discharge hopper (24).
9. Scandium extraction pretreatment system according to claim 1, wherein the fixed bed (30) comprises a barrel (31), a cone (32), a guiding cylinder (33) and a clarification structure (34), wherein the clarification structure (34) is arranged within the barrel (31), the guiding cylinder (33) passes through the clarification structure (34), the cone (32) is located below the barrel (31), the cone (32) and the barrel (31) are in communication, the clarification structure (34) comprises a plurality of resin particles, the second liquid inlet is located in an upper part of the guiding cylinder (33), the second overflow is located in an upper part of the barrel (31), and the second slag discharge is located in a lower part of the cone (32).
10. A method for processing a scandium-containing solution, wherein the method for processing a scandium-containing solution is applied to a scandium extraction pretreatment system according to any one of claims 1 to 9, and the method for processing a scandium-containing solution includes:
feeding a scandium-containing solution and concentrated sulfuric acid into a quenching and tempering section (10) to prepare a quenching and tempering liquid in the quenching and tempering section (10);
feeding the conditioning liquid into an aging settling part (20) for settling solid particles;
the solution overflowed from the aging settling part (20) is conveyed to a fixed bed (30) for filtration, and the filtered solution overflows from the upper part of the aging settling part (20).
11. The method of treatment of a scandium-containing solution according to claim 10, further including:
detecting the turbidity of the solution in the tempering part (10) and the turbidity of the solution in the aging settling part (20);
and adjusting the speed of inputting scandium-containing solution and concentrated sulfuric acid into the tempering part (10) according to the comparison between the turbidity of the solution in the tempering part (10) and the turbidity of the solution in the aging and settling part (20).
12. The method of treatment of a scandium-containing solution according to claim 10, further including:
detecting the temperature of the solution in the aging settling section (20);
adjusting the residence time of the solution in the aging settling section (20) according to the solution temperature in the aging settling section (20).
13. The method of treatment of a scandium-containing solution according to claim 10, further including:
detecting the level of the solution within the fixed bed (30);
when the liquid level of the solution in the fixed bed (30) reaches a preset value, the solution is stopped from being input into the fixed bed (30), and the solution in the fixed bed (30) flows back to an overflow intermediate tank (50).
14. The method of treatment of a scandium-containing solution according to claim 10, further including:
periodically discharging the slurry from the aging settling section (20) and the bottom of the fixed bed (30);
and (3) performing solid-liquid separation on the discharged slurry, and returning the scandium-containing solution obtained after separation to the quenching and tempering section (10).
15. The method of treatment of a scandium-containing solution according to claim 10, wherein,
the mixing mass ratio of the scandium-containing solution to the concentrated sulfuric acid in the quenching and tempering section (10) is 1: 0.01-0.2, wherein the pH value of the tempering liquid is 0.1-2;
the retention time of the solution in the aging settling part (20) is 12-72 h, the solution is naturally cooled to 20-35 ℃, and the turbidity of the solution is reduced by 50-95% after settling;
the turbidity range of the solution overflowing from the fixed bed (30) is 10-100 ppm, and the concentration range of calcium sulfate in the solution is 0.01% -0.1%.
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