Atomizing, mixing, extracting and clarifying device and application thereof in phosphoric acid purification

By designing the multi-track structure and the track clarified layered structure in the phosphoric acid purification process, efficient extraction and continuous operation of phosphoric acid are achieved, and the problems of low extraction efficiency and large equipment area in the existing technology are solved, and the extraction efficiency is improved and operational continuity.

CN119186019AActive Publication Date: 2024-12-27ZHEJIANG UNIV OF TECH
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Patent Information

Application Number
CN202411630409.1
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2024-11-15
Publication Date
2024-12-27
Estimated Expiration
2044-11-15

AI Technical Summary

Technical Problem

The extraction efficiency in the existing phosphoric acid purification process is low, the equipment covers a large area, the inner parts are prone to scale and blockage, and the atomized phosphoric acid droplets accumulate in the extraction tower and affects the extraction effect. The layering clarification time is long, making it difficult to achieve continuous operation. .

Method used

Design atomization and mixed extraction and clarification device, including extraction chambers separated by multiple trays, each chamber is equipped with a nozzle and trays to clarify the layered structure, and the repeated dispersion of the dispersed phase is achieved through continuous atomization of the nozzle and circulating pump. Combined with the tray plate to clarify the layered structure to form stable layering, improving the extraction efficiency and feasibility of continuous operation.

Benefits of technology

It improves the extraction efficiency of the extraction tower, shortens the layered clarification time, realizes continuous operation and amplification of the device, solves the equipment's land occupation and blockage problems, and has good promotion and application prospects.

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Abstract

The invention discloses an atomization mixing extraction clarification device and application thereof in phosphoric acid purification, the device is internally provided with an extraction tower with a plurality of tower plates, the tower plates divide the interior of the extraction tower into n extraction chambers, nozzles are arranged in the upper ends of the first to (n-1) th extraction chambers along the direction from top to bottom, and the nozzles are arranged in the upper ends of the first to (n-1) th extraction chambers. The nozzles in the extraction chambers are connected with the dispersed phase inlets in the side walls of the extraction chambers through pipelines, the dispersed phase outlets of the previous extraction chambers are connected with the dispersed phase inlets of the adjacent next extraction chambers through dispersed phase circulating pumps and pipelines, and the side wall of the upper end of the nth extraction chamber is further provided with a continuous phase inlet; a continuous phase outlet is formed in the top of the first extraction chamber; each tower plate is provided with a tower plate clarification layering structure, and the center of each tower plate clarification layering structure is provided with a channel penetrating through the corresponding tower plate. The nozzles are connected in series, the surface area is greatly increased after dispersed phases are atomized and enter the extraction tower, the dispersed phases are more fully mixed with continuous phases, and the extraction efficiency of the extraction tower is greatly improved.
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Description

Technical Field

[0001] The invention belongs to the technical field of chemical separation, and in particular relates to an atomization mixing extraction clarification device and its application in phosphoric acid purification. Background Art

[0002] Phosphoric acid is widely used in various sectors of the national economy, in washing, food, pharmaceuticals, pigments, electroplating, rust prevention and other industries. Limited by the small amount of high-grade phosphate ore in my country, the cost of phosphoric acid is still high. The development of wet phosphoric acid purification can alleviate this situation. At present, in the field of wet phosphoric acid purification at home and abroad, the main technologies used include extraction, crystallization separation, electrodialysis technology and ion exchange. Among them, extraction is the most widely used wet phosphoric acid purification technology. Compared with other phosphoric acid separation and purification technologies, solvent extraction has the advantages of simple equipment, easy operation and control, low energy consumption, and large production capacity. It is the most widely used method for industrial phosphoric acid purification at home and abroad.

[0003] In Chinese patent CN1654317A, the production process steps of purifying wet-process phosphoric acid by solvent extraction include pretreatment, filtration separation, extraction, washing, stripping and concentration. The process flow is as follows: Figure 1 As shown. The production process pre-treats and filters wet phosphoric acid to remove sulfate and fluoride impurities; then uses an organic solvent to extract phosphoric acid to remove impurities such as sodium salt, potassium salt, and iron salt; the aqueous phase after extraction is the raffinate phase, and the aqueous phase obtained by acid washing and stripping the oil phase after extraction is the purified dilute phosphoric acid; the purified dilute phosphoric acid is concentrated to obtain the phosphoric acid product. Extraction technology can be used in the three key stages of extraction, washing, and stripping in the phosphoric acid purification process. However, in industrial extraction applications, there are problems such as low extraction efficiency, large equipment footprint, and easy scaling and clogging of internal parts.

[0004] Micro-droplet dispersion technology has the advantages of good mass transfer effect and no need for fillers, etc. It can be used for phosphoric acid purification to improve the extraction efficiency. Chinese patent CN219764557 adopts a plurality of atomizing nozzles provided on the side wall of the extraction tower, and the atomizing nozzles are connected to nitrogen pressurization, so that the phosphoric acid is fully atomized before entering the extraction tower, and the atomized phosphoric acid is fully mixed with the extractant after entering the extraction tower. However, the parallel structure of its nozzles makes it easy for the atomized phosphoric acid to aggregate droplets in the extraction tower, which affects the extraction effect, and the concentrated stratification after the atomized phosphoric acid extraction makes the stratification clarification time longer, which is not conducive to the continuous operation of the extraction tower and difficult to scale up. Summary of the invention

[0005] In order to overcome the deficiencies and shortcomings of the prior art, the object of the present invention is to provide an atomization mixing extraction clarification device and its application in phosphoric acid purification. The device of the present invention can effectively improve the extraction efficiency of the extraction tower.

[0006] In order to solve the above technical problems, the technical solution adopted by the present invention is:

[0007] An atomization mixing extraction and clarification device, characterized in that it comprises an extraction tower with a plurality of tower plates arranged inside, the tower plates divide the internal space of the extraction tower into n upper and lower extraction chambers, each extraction chamber has a dispersed phase inlet arranged on the upper side wall, and a dispersed phase outlet arranged on the lower side wall; along the top-to-bottom direction, nozzles are arranged inside the upper ends of the first to n-1 extraction chambers, the nozzles in the extraction chambers are connected to the dispersed phase inlets of the side walls thereof through pipelines, and the dispersed phase outlets of the previous extraction chambers are connected to the adjacent next extraction chambers through pipelines via dispersed phase circulation pumps. The dispersed phase inlet of the chamber allows the dispersed phase liquid in the bottom of the previous extraction chamber to be pumped into the upper end of the adjacent next extraction chamber through a dispersed phase circulation pump and atomized again through a nozzle to disperse into tiny droplets. The upper end side wall of the nth extraction chamber is also provided with a continuous phase inlet, and the top of the first extraction chamber is provided with a continuous phase outlet; wherein a tower plate clarification layered structure is provided on each tower plate, and the center of the tower plate clarification layered structure has a channel penetrating the tower plate, and the continuous phase of the next extraction chamber can enter the adjacent previous extraction chamber through the tower plate clarification layered structure.

[0008] Furthermore, the n is an integer of 3-30.

[0009] Furthermore, along the top-down direction, the dispersed phase inlet of the first extraction chamber is connected to the dispersed phase preheater, the dispersed phase feed pump and the dispersed phase feed tank in sequence through pipelines, and the continuous phase outlet at the top is connected to the continuous phase collection tank through a pipeline.

[0010] Furthermore, along the top-down direction, the continuous phase inlet of the nth extraction chamber is connected to the continuous phase preheater, the continuous phase feed pump and the continuous phase feed tank in sequence through a pipeline, and the dispersed phase outlet at its lower end is connected to the dispersed phase collection tank by a pipeline through a dispersed phase discharge pump.

[0011] Furthermore, the nozzle is a pressure nozzle or a rotary nozzle, the material is stainless steel, plastic or brass, and the aperture is 0.8 to 3.2 mm.

[0012] Furthermore, the number of nozzles in each extraction chamber is multiple, selected from 2-10, preferably 3-5, and the multiple nozzles are arranged in a vertex arrangement of an equilateral triangle or a vertex arrangement of a square.

[0013] Furthermore, the tower plate clarification stratification structure is an internal part of the tower plate, including an intermediate channel pipe with upper and lower openings and a cap. The bottom or lower end side wall of the intermediate channel pipe is fixedly arranged on the tower plate, and the cap is fixed to the intermediate channel pipe by a support rod, and the cap is suspended directly above the upper end opening of the intermediate channel pipe. The dispersed phase droplets fall on the cap, and a stable stratification is formed along the cap in the external area on the edge of the intermediate channel pipe.

[0014] Furthermore, a sight glass is provided on the side of the extraction tower, and the dispersed phase inlets of the other extraction chambers except the top extraction chamber are all arranged close to the tower plate, and the dispersed phase outlets of the other extraction chambers except the bottom extraction chamber are all arranged close to the tower plate; in the same extraction chamber, the height of the dispersed phase outlet is smaller than the height of the upper end opening of the intermediate channel pipe.

[0015] The process method of the atomization mixing extraction clarification device comprises the following steps:

[0016] 1) The continuous phase is the light phase and the dispersed phase is the heavy phase. The continuous phase is introduced from the continuous phase inlet of the bottom extraction chamber, passes through the plate from bottom to top through the central channel of the plate clarification layered structure into the adjacent extraction chamber, and so on, finally enters the top extraction chamber and is discharged from the continuous phase outlet;

[0017] 2) The dispersed phase is introduced from the dispersed phase inlet of the top extraction chamber, atomized at the nozzle, and dispersed into tiny droplets. The dispersed phase tiny droplets settle downward and form a layer with the continuous phase in the outer area of ​​the tower plate clarification layer structure. The dispersed phase layer settles on the tower plate, is pumped out by the dispersed phase circulation pump and introduced into the upper end of the next adjacent extraction chamber, and is atomized again by the nozzle to disperse into tiny droplets. After multiple cycles, it finally enters the bottom extraction chamber and is discharged from the dispersed phase outlet.

[0018] Furthermore, the device is applied to the extraction, washing or stripping section in the phosphoric acid purification process.

[0019] Furthermore, the temperature in the extraction tower is 40-80° C., preferably 60-80° C., the spacing between the tower plates is 0.4-1.2 m, preferably 0.8-1.2 m, the dispersed phase raw material is a phosphoric acid solution with a mass fraction of 20-80%, the continuous phase includes an extractant, the extractant is one of tributyl phosphate, methyl isobutyl ketone or isoamyl alcohol, and when the extractant is tributyl phosphate or methyl isobutyl ketone, it is diluted with a low-viscosity weak polar solvent, the low-viscosity weak polar solvent is at least one of kerosene, C6-C8 alkane, diisopropyl ether or isoamyl alcohol, the volume ratio of the extractant to the low-viscosity non-polar solvent is 2-5:1, and the volume flow ratio of the continuous phase to the dispersed phase raw material is 1-6, preferably 2-4:1.

[0020] Beneficial effects of the present invention:

[0021] 1. After atomization, the droplet size of the dispersed phase is reduced, the specific surface area is increased, and the contact and mixing with the continuous phase are more complete, which greatly improves the extraction efficiency of the extraction tower;

[0022] 2. The multi-layer nozzles are connected in series. After the dispersed phase is atomized and enters the extraction tower, the surface area is greatly increased and the continuous phase is mixed more fully, which greatly improves the extraction efficiency of the extraction tower. In addition, the dispersed phase can be repeatedly atomized, and the dispersed phase droplets can be atomized and dispersed again after they gather and become larger, thereby further improving the extraction efficiency.

[0023] 3. A new tray clarification layered structure is adopted. The tray clarification layered structure is a tray internal, including a middle channel pipe with upper and lower openings and a cap. The dispersed phase droplets fall on the cap and form a stable layer along the outer area of ​​the middle channel pipe along the cap, shortening the overall layer clarification time;

[0024] 4. The process flow of the present invention is simple, and no tower internals such as fillers are required. It is easy to realize continuous operation and device enlargement, and has good prospects for promotion and application. BRIEF DESCRIPTION OF THE DRAWINGS

[0025] Figure 1 It is a process flow chart of wet phosphoric acid extraction and purification;

[0026] Figure 2 It is a structural schematic diagram of an atomization mixing extraction and clarification device of the present invention;

[0027] Figure 2 In: 1-continuous phase feed tank, 2-continuous phase feed pump, 3-continuous phase preheater, 4-dispersed phase feed tank, 5-dispersed phase feed pump, 6-dispersed phase preheater, 7-nozzle, 8-extraction tower, 9-plate clarification layered structure, 10-dispersed phase circulation pump, 11-continuous phase collection tank, 12-dispersed phase discharge pump, 13-dispersed phase collection tank, 8-1 is the continuous phase inlet, 8-2 is the continuous phase outlet, 8-3 is the dispersed phase inlet, 8-4 is the dispersed phase outlet, and 8-5 is the vent valve.

[0028] Figure 3 It is a schematic diagram of the regular triangle arrangement and square arrangement of nozzles of an atomization mixing extraction and clarification device of the present invention;

[0029] Figure 3 Middle: 7-nozzle;

[0030] Figure 4 This is a schematic diagram of a plate clarification layered structure of an atomization mixing extraction clarification device of the present invention.

[0031] Figure 4 Middle: 9-a is a cap, and 9-b is a middle channel pipe fitting. DETAILED DESCRIPTION

[0032] The present invention will be further described below in conjunction with specific embodiments, but the protection scope of the present invention is not limited thereto.

[0033] Example:

[0034] An atomization mixing extraction and clarification device includes an extraction tower 8 with a plurality of trays arranged therein, wherein the trays divide the inner space of the extraction tower 8 into n upper and lower extraction chambers, where n is an integer ≥ 3, for example Figure 2 In the structure, n=4. A dispersed phase inlet 8-3 is arranged on the upper side wall of each extraction chamber, and a dispersed phase outlet 8-4 is arranged on the lower side wall; along the direction from top to bottom, nozzles 7 are arranged inside the upper ends of the 1st to n-1th extraction chambers, and the nozzles 7 in the extraction chambers are connected to the dispersed phase inlet 8-3 of the side wall thereof through pipelines, and the dispersed phase outlet 8-4 of the previous extraction chamber is connected to the dispersed phase inlet 8-3 of the adjacent next extraction chamber through a dispersed phase circulation pump 10 through a pipeline, so that the dispersed phase liquid in the bottom of the previous extraction chamber is pumped into the upper end of the adjacent next extraction chamber through the dispersed phase circulation pump 10 and is atomized and dispersed into tiny droplets again through the nozzle 7, and a continuous phase inlet 8-1 is also arranged on the upper side wall of the nth extraction chamber, and a continuous phase outlet 8-2 is arranged on the top of the first extraction chamber; wherein a plate clarification layered structure 9 is arranged on each plate, and a channel penetrating the plate is provided in the center of the plate clarification layered structure 9, and the continuous phase of the next extraction chamber can enter the adjacent previous extraction chamber through the plate clarification layered structure 9.

[0035] Comparison Figure 2 In the embodiment, a vent valve 8-5 is also provided at the top of the first extraction chamber.

[0036] Comparison Figure 2 , along the top-down direction, the dispersed phase inlet 8-3 of the first extraction chamber is connected to the dispersed phase preheater 6, the dispersed phase feed pump 5 and the dispersed phase feed tank 4 in sequence through pipelines, and the continuous phase outlet 8-2 at the top is connected to the continuous phase collection tank 11 through pipelines. The continuous phase inlet 8-1 of the nth extraction chamber is connected to the continuous phase preheater 3, the continuous phase feed pump 2 and the continuous phase feed tank 1 in sequence through pipelines, and the dispersed phase outlet 8-4 at the lower end is connected to the dispersed phase collection tank 13 through a dispersed phase discharge pump 12 by a pipeline.

[0037] The nozzle type is a pressure nozzle or a rotary nozzle, and the material is stainless steel, plastic or brass, and the aperture is 0.8 to 3.2 mm. The number of nozzles is multiple, and the arrangement of multiple nozzles is a vertex arrangement of an equilateral triangle or a vertex arrangement of a square. The schematic diagram of the nozzle arrangement structure is as follows Figure 3 shown.

[0038] Comparison Figure 4In the figure, the tower plate clarification stratification structure 9 is an internal part of the tower plate, including an intermediate channel pipe 9-b with upper and lower openings and a cap 9-a. The bottom or lower end side wall of the intermediate channel pipe 9-b is fixedly arranged on the tower plate, and the cap 9-a is fixed to the intermediate channel pipe 9-b by a support rod, and the cap 9-a is suspended directly above the upper end opening of the intermediate channel pipe 9-b. The dispersed phase droplets fall on the cap, and a stable stratification is formed along the cap in the external area on the edge of the intermediate channel pipe 9-b.

[0039] A sight glass is provided on the side of the extraction tower 8. The dispersed phase inlets 8-3 of the extraction chambers other than the top extraction chamber are all arranged close to the tower plate, and the dispersed phase outlets 8-4 of the extraction chambers other than the bottom extraction chamber are all arranged close to the tower plate; in the same extraction chamber, the height of the dispersed phase outlet 8-4 is smaller than the height of the upper opening of the intermediate channel pipe 9-b.

[0040] An atomization mixing extraction and clarification device can be used for Figure 1 The extraction, washing and stripping sections in the phosphoric acid purification process are shown.

[0041] Examples 1 to 12

[0042] According to Figure 2 The device shown is used for the extraction section in phosphoric acid purification:

[0043] 1) Wet-process phosphoric acid to be extracted is used as a dispersed phase, wherein the phosphoric acid is an aqueous phase solution with a mass fraction of 65%, wherein the impurities sodium sulfate have a mass fraction of 4.5%, potassium sulfate have a mass fraction of 5.2%, calcium sulfate have a mass fraction of 0.44%, and lead sulfate have a mass fraction of 0.16%; the continuous phase is a mixture of an extractant and a diluent, wherein the extractant is tributyl phosphate, and the diluent is kerosene, and the tributyl phosphate and kerosene are mixed in a volume ratio of 4:1, and the volume flow ratio of the continuous phase to the dispersed phase is the extraction phase ratio.

[0044] 2) The inner diameter of the extraction tower 8 is 0.6 m, and 6 trays are arranged in the tower, and each tray is provided with a tray clarification layered structure 9. The 6 trays divide the interior of the extraction tower 8 into 7 extraction chambers, and the distance between adjacent trays is 0.4 to 1.2 m. From top to bottom, 3 nozzles 7 are arranged inside the upper ends of the 1st to 6th extraction chambers, and the nozzles are arranged in the three vertices of an equilateral triangle. The nozzle material is stainless steel 316L, and the aperture is 1 mm;

[0045] 3) Add the extractant into the continuous phase feed tank 1, and the continuous phase is delivered by the continuous phase feed pump 2, with the flow rate set at 7.5-30 L / min, passes through the continuous phase preheater 3, and the extraction temperature is set at 40-80° C., enters the bottom side of the extraction tower 8, and passes through the tower plate from bottom to top through the central channel of the tower plate clarification layered structure 9 into the adjacent extraction chamber, and so on, and finally enters the top extraction chamber and is discharged from the continuous phase outlet 8-2 to the outside, and enters the continuous phase collection tank 11;

[0046] 4) The phosphoric acid to be extracted is added to the dispersed phase feed tank 4, and the dispersed phase is transported by the dispersed phase feed pump 5, with the flow rate set to 7.5 L / min, and passes through the dispersed phase preheater 6, and the extraction temperature is set to 40-80° C., and is introduced from the dispersed phase inlet 8-3 of the uppermost extraction chamber, atomized at the nozzle 7, and dispersed into tiny droplets. The tiny droplets form a layer with the continuous phase in the outer area of ​​the tower plate clarification layer structure 9, and the dispersed phase layer settles on the tower plate, is pumped out by the dispersed phase circulation pump 10 and introduced into the upper end of the adjacent next extraction chamber, and is atomized again by the nozzle 7 to disperse into tiny droplets. After multiple cycles, it finally enters the lowermost extraction chamber and is discharged outward from the dispersed phase outlet 8-4, and is pumped out by the dispersed phase discharge pump 12 into the dispersed phase collection tank 13.

[0047] The continuous extraction is carried out according to the experimental steps of step 1) to step 4), and the extraction efficiency is calculated when the extraction is stable. Extraction efficiency = the amount of phosphoric acid collected in the continuous phase collection tank 11 / the amount of phosphoric acid output from the dispersed phase feed tank 4.

[0048] In addition, the extraction clarification time of the dispersed phase in the continuous phase in the extraction chamber is also tested. The testing method is: carry out continuous extraction according to the experimental steps of the above steps 1) to 4). When the extraction is stable, stop the introduction and discharge of the dispersed phase and the continuous phase in the extraction tower 8, and carry out static stratification. Observe that from the moment of stopping, the dispersed phase in the extraction chamber is completely settled in the continuous phase to form a clear upper and lower stratification phenomenon. The time consumed is the extraction clarification time described in this application.

[0049] According to the above experimental process, the extraction temperature, continuous phase flow rate, adjacent plate spacing and other parameter conditions in Examples 1-12, as well as the results of the tested extraction efficiency and extraction clarification time are listed in Table 1.

[0050] Table 1. Comparison of phosphoric acid extraction efficiency under different process conditions

[0051]

[0052] It can be seen from Table 1 that good extraction effect can be achieved when the extraction temperature is 60-80°C, the extraction ratio is 1-4, and the distance between adjacent tower plates is 0.8-1.2m.

[0053] Comparative Examples 1 to 3

[0054] According to Figure 2 The device shown in the figure is used for the extraction section in the purification of phosphoric acid. The experimental steps are the same as the experimental conditions in Example 3, with the only difference that "the nozzle 7 in the extraction chamber is replaced by a feed pipe with an inner diameter of 1 to 3 mm and a length of 0.2 m, and the feed pipe is arranged in the three vertices of a regular triangle", the extraction temperature is 60°C, the continuous phase flow rate is 30 L / min, the extraction phase ratio is 4, and the tower plate spacing is 1 m. The experimental results are summarized in Table 2.

[0055] Table 2. Comparison of extraction efficiency of different feed tube inner diameters

[0056] name Feed pipe inner diameter, mm Extraction efficiency, % Extraction clarification time, min Comparative Example 1 1 75.6 17.2 Comparative Example 2 2 73.8 17.5 Comparative Example 3 3 70.6 17.7

[0057] Comparative Example 4

[0058] A tower type extraction mixing and clarification device is used, with an extractant feed pipe and a raffinate discharge pipe on the bottom side, an extractant discharge pipe on the top side, and 48 evenly distributed atomizing nozzles on the side wall, the nozzle material is stainless steel 316L, and the aperture is 1mm. The composition of the phosphoric acid to be extracted is the same as that in Example 1, the continuous phase is a mixture of an extractant and a diluent, the extractant is tributyl phosphate, the diluent is kerosene, and tributyl phosphate and kerosene are mixed in a volume ratio of 4:1. The extraction phase ratio is 4, the extraction tower body is designed to be 7m, and the inner diameter of the tower is 0.6m. The continuous phase solution is added to the extractant feed tank, and the continuous phase solution is transported by the extractant feed pump, with a set flow rate of 30L / min, passing through the extractant preheater, with a set temperature of 60°C, and entering the bottom side of the extraction tower from the extractant feed pipeline; the phosphoric acid to be extracted is added to the phosphoric acid feed tank, and the phosphoric acid is transported by the phosphoric acid feed pump, with a set flow rate of 7.5L / min, passing through the phosphoric acid preheater, with a set temperature of 60°C, atomized at the nozzle on the side wall of the extraction tower, dispersed into tiny droplets, fully mixed with the extractant in the tower, and finally from the outlet below the extraction tower through the raffinate discharge pump and the raffinate discharge pipeline into the raffinate bottom tank. The extractant moves to the top of the extraction tower by its own buoyancy, and contacts the atomized and dispersed phosphoric acid in reverse, and finally forms a saturated liquid that is discharged from the top of the extraction tower and enters the extraction liquid bottom tank.

[0059] Finally, the phosphoric acid extraction efficiency was 72.4% and the extraction settlement time was 38 min.

[0060] Comparative Example 5

[0061] According to Figure 2The device shown in the figure is used for the extraction section in the purification of phosphoric acid. The experimental steps are the same as those in Example 3, except that "the tower internals with a sieve plate with a pore size of 5 mm are used instead of the tower plate with a tower plate clarification layered structure 9", the extraction temperature is 60°C, the continuous phase flow rate is 30L / min, the extraction phase ratio is 4, and the tower plate spacing is 1m. Finally, the phosphoric acid extraction efficiency is 63.6%, and the extraction clarification time is 45min.

[0062] The contents described in this specification are merely an enumeration of implementation forms of the inventive concept, and the protection scope of the present invention should not be regarded as being limited to the specific forms described in the embodiments.

Claims

1. An atomization mixing extraction clarification device, characterized in that An extraction tower (8) is provided with a plurality of tower plates, wherein the tower plates divide the internal space of the extraction tower (8) into n upper and lower extraction chambers, wherein a dispersed phase inlet (8-3) is provided on the upper side wall of each extraction chamber, and a dispersed phase outlet (8-4) is provided on the lower side wall; along the top-to-bottom direction, nozzles (7) are provided inside the upper ends of the first to n-1 extraction chambers, wherein the nozzles (7) in the extraction chambers are connected to the dispersed phase inlet (8-3) on the side wall thereof via pipelines, and the dispersed phase outlet (8-4) of the previous extraction chamber is connected to the dispersed phase outlet (8-4) of the next adjacent extraction chamber via pipelines via dispersed phase circulation pumps (10). The inlet (8-3) allows the dispersed phase liquid in the bottom of the previous extraction chamber to be pumped into the upper end of the adjacent next extraction chamber through the dispersed phase circulation pump (10) and atomized and dispersed into tiny droplets again through the nozzle (7). The upper end side wall of the nth extraction chamber is also provided with a continuous phase inlet (8-1), and the top of the first extraction chamber is provided with a continuous phase outlet (8-2); wherein a plate clarification layered structure (9) is provided on each plate, and the center of the plate clarification layered structure (9) has a channel penetrating the plate, and the continuous phase of the next extraction chamber can enter the adjacent previous extraction chamber through the plate clarification layered structure (9).

2. The atomization mixing extraction and clarification device according to claim 1, characterized in that Along the top-down direction, the dispersed phase inlet (8-3) of the first extraction chamber is connected to the dispersed phase preheater (6), the dispersed phase feed pump (5) and the dispersed phase feed tank (4) in sequence through pipelines, and the continuous phase outlet (8-2) at the top is connected to the continuous phase collection tank (11) through a pipeline; n is an integer of 3-30.

3. The atomization mixing extraction and clarification device according to claim 1, characterized in that In a top-down direction, the continuous phase inlet (8-1) of the nth extraction chamber is connected to the continuous phase preheater (3), the continuous phase feed pump (2) and the continuous phase feed tank (1) in sequence through pipelines, and the dispersed phase outlet (8-4) at its lower end is connected to the dispersed phase collection tank (13) through a dispersed phase discharge pump (12) through a pipeline.

4. The atomization mixing extraction and clarification device according to claim 1, characterized in that The nozzle type is a pressure nozzle or a rotary nozzle, the material is stainless steel, plastic or brass, and the aperture is 0.1~3.0 mm.

5. The atomization mixing extraction and clarification device according to claim 1, characterized in that The number of nozzles in each extraction chamber is multiple, selected from 2-10, preferably 3-5, and the arrangement of the multiple nozzles is a vertex arrangement of an equilateral triangle or a vertex arrangement of a square.

6. The atomization mixing extraction and clarification device according to claim 1, characterized in that The tower plate clarifying layering structure (9) is an internal part of the tower plate, comprising an intermediate channel pipe (9-b) with upper and lower openings and a cap (9-a), wherein the bottom or lower end side wall of the intermediate channel pipe (9-b) is fixedly arranged on the tower plate, and the cap (9-a) is fixed to the intermediate channel pipe (9-b) by a support rod, and the cap (9-a) is suspended directly above the upper end opening of the intermediate channel pipe (9-b), and dispersed phase droplets fall on the cap, and a stable layer is formed along the cap in the outer area on the edge of the intermediate channel pipe (9-b).

7. The atomization mixing extraction and clarification device according to claim 6, characterized in that The extraction tower (8) is provided with a sight glass on the side, and the dispersed phase inlets (8-3) of the other extraction chambers except the top extraction chamber are all arranged close to the tower plate, and the dispersed phase outlets (8-4) of the other extraction chambers except the bottom extraction chamber are all arranged close to the tower plate; in the same extraction chamber, the height of the dispersed phase outlet (8-4) is less than the height of the upper end opening of the intermediate channel pipe (9-b).

8. The process of the atomization mixing extraction and clarification device according to claim 1, characterized in that The following steps are involved: 1) The continuous phase is the light phase and the dispersed phase is the heavy phase. The continuous phase is introduced from the continuous phase inlet (8-1) of the bottom extraction chamber, passes through the plate from bottom to top through the central channel of the plate clarification layered structure (9) into the adjacent extraction chamber, and so on, finally enters the top extraction chamber and is discharged from the continuous phase outlet (8-2); 2) The dispersed phase is introduced from the dispersed phase inlet (8-3) of the top extraction chamber, atomized at the nozzle (7), and dispersed into tiny droplets. The dispersed phase tiny droplets settle downward and form a layer with the continuous phase in the outer area of ​​the tower plate clarification layer structure (9). The dispersed phase layer settles on the tower plate, is pumped out by the dispersed phase circulation pump (10) and introduced into the upper end of the next adjacent extraction chamber, where it is atomized again by the nozzle (7) and dispersed into tiny droplets. After multiple cycles, it finally enters the bottom extraction chamber and is discharged from the dispersed phase outlet (8-4).

9. The process of the atomization mixing extraction clarification device according to claim 8, characterized in that The device is applied to the extraction, washing or stripping section in the phosphoric acid purification process.

10. The process of the atomization mixing extraction clarification device according to claim 8, characterized in that The temperature in the extraction tower (8) is 40-80°C, preferably 60-80°C, the distance between the tower plates is 0.4-1.2 m, preferably 0.8-1.2 m, the dispersed phase raw material is a phosphoric acid solution with a mass fraction of 20-80%, the continuous phase comprises an extractant, the extractant is one of tributyl phosphate, methyl isobutyl ketone or isoamyl alcohol, when the extractant is tributyl phosphate or methyl isobutyl ketone, it is diluted with a low-viscosity weak polar solvent, the low-viscosity weak polar solvent is at least one of kerosene, C6-C8 alkane, diisopropyl ether or isoamyl alcohol, the volume ratio of the extractant to the low-viscosity non-polar solvent is 2-5:1, and the volume flow ratio of the continuous phase to the dispersed phase raw material is 1-6, preferably 2-4:1.

Citation Information

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