An atomizing mixing extraction clarification device and its application in phosphoric acid purification

By employing an atomizing mixing extraction clarification device with multi-layer nozzle series connection and tray clarification layer structure in the phosphoric acid purification process, the problems of low extraction efficiency and equipment blockage are solved, achieving efficient phosphoric acid purification and continuous operation of the device.

CN119186019BActive Publication Date: 2026-04-21ZHEJIANG UNIV OF TECH
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
ZHEJIANG UNIV OF TECH
Filing Date
2024-11-15
Publication Date
2026-04-21

AI Technical Summary

Technical Problem

Existing phosphoric acid purification processes suffer from low extraction efficiency, large equipment footprint, and easy scaling and clogging of internal components. Furthermore, atomized phosphoric acid tends to aggregate in the extraction tower, affecting the efficiency and making it difficult to achieve continuous operation and scale-up of the equipment.

Method used

A multi-layer nozzle series-connected atomizing mixing extraction clarification device is used. The extraction tower is divided into multiple extraction chambers by setting multiple trays. Each chamber is equipped with a nozzle and a dispersed phase inlet at the top. The dispersed phase is atomized multiple times by using a dispersed phase circulation pump. Combined with the tray clarification layer structure, the mixing efficiency of the dispersed phase and the continuous phase is improved.

Benefits of technology

It significantly improves the extraction efficiency of the extraction tower, shortens the stratification time, enables continuous operation of the device and easy scale-up, and reduces the equipment footprint.

✦ Generated by Eureka AI based on patent content.

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Abstract

This invention discloses an atomizing mixing extraction clarification device and its application in phosphoric acid purification. The device comprises an extraction tower with multiple trays, dividing the tower into n extraction chambers. From top to bottom, nozzles are installed at the upper end of the first to (n-1)th extraction chambers. Each nozzle is connected to a dispersed phase inlet on its sidewall via piping. The dispersed phase outlet of each previous extraction chamber is connected to the dispersed phase inlet of the next adjacent extraction chamber via a dispersed phase circulation pump. A continuous phase inlet is also provided on the upper sidewall of the nth extraction chamber, and a continuous phase outlet is located at the top of the first extraction chamber. Each tray has a tray clarification layer structure with a channel penetrating the center. This invention connects the nozzles in series, significantly increasing the surface area of ​​the dispersed phase after atomization into the extraction tower and ensuring more thorough mixing with the continuous phase, thereby greatly improving the extraction efficiency of the extraction tower.
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Description

Technical Field

[0001] This invention belongs to the field of chemical separation technology, specifically relating to an atomizing mixing extraction clarification device and its application in phosphoric acid purification. Background Technology

[0002] Phosphoric acid is widely used in various sectors of the national economy, including detergents, food, pharmaceuticals, pigments, electroplating, and rust prevention. However, due to the scarcity of high-grade phosphate rock in my country, the cost of phosphoric acid remains relatively high. Developing wet-process phosphoric acid purification can alleviate this situation. Currently, the main technologies used in the domestic and international wet-process phosphoric acid purification field include extraction, crystallization separation, electrodialysis, and ion exchange. Among these, extraction is the most widely used wet-process phosphoric acid purification technology. Compared with other phosphoric acid separation and purification technologies, solvent extraction has advantages such as simple equipment, easy operation and control, low energy consumption, and large production capacity, making it the most widely used method for industrial phosphoric acid purification both domestically and internationally.

[0003] In Chinese patent CN1654317A, the production process of purifying chemical wet-process phosphoric acid by solvent extraction includes, in sequence, pretreatment, filtration and separation, extraction, washing, back-extraction, and concentration. The process flow is as follows: Figure 1 As shown in the diagram, this production process pretreats and filters wet-process phosphoric acid to remove sulfate and fluoride impurities. Then, it extracts the phosphoric acid with an organic solvent to remove sodium, potassium, and iron salts. The aqueous phase after extraction is the raffinate, and the oil phase after extraction is acid-washed and back-extracted to obtain the purified dilute phosphoric acid. The purified dilute phosphoric acid is then concentrated to obtain the final phosphoric acid product. Extraction technology can be used in the three key stages of phosphoric acid purification: extraction, washing, and back-extraction. However, industrial extraction applications suffer from problems such as low extraction efficiency, large equipment footprint, and easy scaling and clogging of internal components.

[0004] Microdroplet dispersion technology offers advantages such as good mass transfer and no need for packing materials, and can improve extraction efficiency in phosphoric acid purification. Chinese patent CN219764557 employs multiple atomizing nozzles on the sidewall of the extraction tower, connected to nitrogen pressurization, to ensure that the phosphoric acid is fully atomized before entering the extraction tower, and that the atomized phosphoric acid is thoroughly mixed with the extractant after entering the tower. However, the parallel structure of the nozzles makes the atomized phosphoric acid prone to droplet coalescence in the extraction tower, affecting the extraction effect. Furthermore, the concentrated stratification after extraction results in a long stratification time, which is detrimental to the continuous operation of the extraction tower and makes scale-up difficult. Summary of the Invention

[0005] In order to overcome the shortcomings and disadvantages of the existing technology, the purpose of this invention is to provide an atomizing mixing extraction clarification device and its application in phosphoric acid purification. The device of this invention can effectively improve the extraction efficiency of the extraction tower.

[0006] To solve the above-mentioned technical problems, the technical solution adopted by the present invention is as follows:

[0007] Atomizing mixing extraction and clarification device is characterized by comprising an extraction tower with multiple trays inside, the trays dividing the internal space of the extraction tower into n upper and lower extraction chambers. Each extraction chamber has a dispersed phase inlet on its upper sidewall and a dispersed phase outlet on its lower sidewall. From top to bottom, nozzles are provided inside the upper part of the first to (n-1)th extraction chambers. The nozzles in the extraction chambers are connected to the dispersed phase inlets on their sidewalls via pipelines. The dispersed phase outlets of the previous extraction chambers are connected to the next adjacent extraction chamber via dispersed phase circulation pumps via pipelines. The dispersed phase inlet of the chamber allows the dispersed phase liquid at the bottom of the previous extraction chamber to be pumped into the upper part of the next adjacent extraction chamber by a dispersed phase circulation pump and then atomized and dispersed into tiny droplets again by a nozzle. The upper 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. Each tray is provided with a tray clarification layer structure, and the center of the tray clarification layer structure has a channel that penetrates through the tray. The continuous phase of the next extraction chamber can enter the next adjacent extraction chamber through the tray clarification layer structure.

[0008] Furthermore, n is an integer between 3 and 30.

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

[0010] Furthermore, along the top-to-bottom direction, the continuous phase inlet of the nth extraction chamber is sequentially connected to the continuous phase preheater, the continuous phase feed pump, and the continuous phase feed tank via pipelines, and the dispersed phase outlet at its lower end is connected to the dispersed phase collection tank via a dispersed phase discharge pump via pipelines.

[0011] Furthermore, the nozzle type is a pressure nozzle or a rotary nozzle, and the material is stainless steel, plastic or brass, with an orifice diameter of 0.8 to 3.2 mm.

[0012] Furthermore, the number of nozzles in each extraction chamber is multiple, selected from 2 to 10, preferably 3 to 5, and the multiple nozzles are arranged in the form of equilateral triangles or squares.

[0013] Furthermore, the clarified stratification structure of the tray is an internal component of the tray, including an intermediate channel pipe with openings at the top and bottom and a cap. The bottom or lower side wall of the intermediate channel pipe is fixedly installed on the tray, and the cap is fixed to the intermediate channel pipe by a support rod. The cap is suspended directly above the upper opening of the intermediate channel pipe. The dispersed liquid drops fall onto the cap and form a stable stratification along the cap in the outer area of ​​the intermediate channel pipe.

[0014] Furthermore, the extraction tower is equipped with a sight glass on its side. The dispersed phase inlets of the extraction chambers other than the uppermost extraction chamber are all located close to the tower plate, and the dispersed phase outlets of the extraction chambers other than the lowermost extraction chamber are all located close to the tower plate. In the same extraction chamber, the height of the dispersed phase outlet is less than the height of the upper opening of the intermediate channel pipe.

[0015] The process method of the atomizing mixing extraction clarification device includes 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, and enters the adjacent extraction chamber from the bottom up through the central channel of the clarified layer structure of the tray, and so on, and 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 uppermost extraction chamber, atomized at the nozzle, and dispersed into tiny droplets. The tiny droplets of the dispersed phase settle downwards and form a stratification with the continuous phase in the outer region of the clarified stratification structure of the tray. The dispersed phase layer settles on the tray and is pumped out by the dispersed phase circulation pump and introduced into the upper end of the next adjacent extraction chamber, where it is atomized and dispersed into tiny droplets again by the nozzle. After multiple cycles, it finally enters the lowermost extraction chamber and is discharged outwards from the dispersed phase outlet.

[0018] Furthermore, the device is applied to the extraction, washing, or back-extraction stages in the phosphoric acid purification process.

[0019] Further, the temperature inside the extraction tower is 40-80℃, preferably 60-80℃, the tray spacing is 0.4-1.2m, preferably 0.8-1.2m, the dispersed phase feedstock is a phosphoric acid solution with a mass fraction of 20-80%, the continuous phase includes an extractant, which 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, weakly polar solvent, which is at least one of kerosene, C6-C8 alkanes, 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 feedstock is 1-6, preferably 2-4:1.

[0020] Beneficial effects of this invention:

[0021] 1. After atomization, the dispersed phase has a smaller droplet size and a larger specific surface area, resulting in more thorough mixing with the continuous phase and greatly improving the extraction efficiency of the extraction tower;

[0022] 2. By connecting multiple nozzles in series, the surface area of ​​the dispersed phase increases significantly after it enters the extraction tower, and the mixing with the continuous phase is more thorough, which greatly improves the extraction efficiency of the extraction tower. In addition, the dispersed phase can be repeatedly atomized. After the dispersed phase droplets coalesce and become larger, they can be atomized and dispersed again, thereby further improving the extraction efficiency.

[0023] 3. A new tray clarification and stratification structure is adopted. The tray clarification and stratification structure consists of tray internals, including a middle channel pipe with openings at the top and bottom and a cap. The dispersed liquid droplets fall onto the cap and form a stable stratification along the outer area of ​​the middle channel pipe, thus shortening the overall stratification and clarification time.

[0024] 4. The process of this invention is simple and does not require tower internals such as packing, making it easy to achieve continuous operation and scale-up of the equipment, and has good prospects for promotion and application. Attached Figure Description

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

[0026] Figure 2 This is a schematic diagram of the structure of an atomizing mixing extraction and clarification device according to the present invention;

[0027] Figure 2 In the middle section: 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-Tray clarification and stratification 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 This is a schematic diagram of the nozzles of an atomizing mixing extraction clarification device of the present invention, showing an equilateral triangle arrangement and a square arrangement;

[0029] Figure 3 7- Nozzle;

[0030] Figure 4 This is a schematic diagram of the tray clarification and layering structure of an atomizing mixing extraction clarification device according to the present invention.

[0031] Figure 4 In the middle: 9-a is the cap, and 9-b is the middle channel fitting. Detailed Implementation

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

[0033] Example:

[0034] An atomizing mixing extraction clarification device includes an extraction tower 8 with multiple trays inside, the trays dividing the internal 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. Each extraction chamber has a dispersed phase inlet 8-3 on its upper sidewall and a dispersed phase outlet 8-4 on its lower sidewall. From top to bottom, nozzles 7 are installed inside the upper part of the first to (n-1)th extraction chambers. The nozzles 7 within the extraction chambers are connected to the dispersed phase inlets 8-3 on their sidewalls via pipelines. The dispersed phase outlets 8-4 of the previous extraction chamber are connected to the dispersed phase inlets 8-3 of the next adjacent extraction chamber via a dispersed phase circulation pump 10. This allows the dispersed phase liquid at the bottom of the previous extraction chamber to be pumped by the dispersed phase circulation pump 10 into the upper part of the next adjacent extraction chamber, where it is atomized and dispersed again into tiny droplets by the nozzles 7. A continuous phase inlet 8-1 is also installed on the upper sidewall of the nth extraction chamber, and a continuous phase outlet 8-2 is installed at the top of the first extraction chamber. Each tray has a tray clarification and layering structure 9, with a channel penetrating the tray at its center. The continuous phase from the next extraction chamber can enter the adjacent previous extraction chamber through the tray clarification and layering structure 9.

[0035] Comparison Figure 2 In the middle, the top of the first extraction chamber is also equipped with a vent valve 8-5.

[0036] Comparison Figure 2 Along the top-to-bottom direction, the dispersed phase inlet 8-3 of the first extraction chamber is connected in sequence to the dispersed phase preheater 6, the dispersed phase feed pump 5, and the dispersed phase feed tank 4 via pipelines. Its top continuous phase outlet 8-2 is connected to the continuous phase collection tank 11 via pipelines. The continuous phase inlet 8-1 of the nth extraction chamber is connected in sequence to the continuous phase preheater 3, the continuous phase feed pump 2, and the continuous phase feed tank 1 via pipelines. Its lower dispersed phase outlet 8-4 is connected to the dispersed phase collection tank 13 via the dispersed phase discharge pump 12 via pipelines.

[0037] The nozzles are either pressure nozzles or rotary nozzles, made of stainless steel, plastic, or brass, with an orifice diameter of 0.8–3.2 mm. Multiple nozzles are used, arranged in either an equilateral triangle or a square configuration. A schematic diagram of the nozzle arrangement is shown below. Figure 3 As shown.

[0038] Comparison Figure 4In the tray, the clarifying and stratifying structure 9 is an internal component of the tray, including an intermediate channel pipe 9-b with openings at the top and bottom and a cap 9-a. The bottom or lower side wall of the intermediate channel pipe 9-b is fixed on the tray. The cap 9-a is fixed to the intermediate channel pipe 9-b by a support rod and is suspended directly above the upper opening of the intermediate channel pipe 9-b. The dispersed liquid drops fall onto the cap and form a stable stratification along the cap in the outer area of ​​the intermediate channel pipe 9-b.

[0039] The extraction tower 8 is equipped with a sight glass on its side. The dispersed phase inlets 8-3 of the extraction chambers other than the uppermost extraction chamber are all located close to the tower plate. The dispersed phase outlets 8-4 of the extraction chambers other than the lowermost extraction chamber are all located 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 opening of the intermediate channel fitting 9-b.

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

[0041] Examples 1-12

[0042] According to such Figure 2 The apparatus shown is used for the extraction stage in phosphoric acid purification.

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

[0044] 2) The extraction tower 8 has an inner diameter of 0.6m and is equipped with 6 trays. Each tray is equipped with a clarification and stratification structure 9. The 6 trays divide the interior of the extraction tower 8 into 7 extraction chambers. The distance between adjacent trays is 0.4 to 1.2m. Along the top-to-bottom direction, the upper end of the 1st to 6th extraction chambers is equipped with 3 nozzles 7. The nozzles are arranged in the form of three vertices of an equilateral triangle. The nozzles are made of 316L stainless steel and have an orifice diameter of 1mm.

[0045] 3) Add the extractant to the continuous phase feed tank 1. The continuous phase is conveyed by the continuous phase feed pump 2 with a flow rate of 7.5-30 L / min. After passing through the continuous phase preheater 3, the extraction temperature is set to 40-80℃. The extractant enters the bottom side of the extraction tower 8 and enters the adjacent extraction chamber from the center channel of the clarification and stratification structure 9 of the tower plate from bottom to top. This process continues until the extractant enters the uppermost extraction chamber and is discharged from the continuous phase outlet 8-2 into the continuous phase collection tank 11.

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

[0047] Perform continuous extraction according to the experimental steps 1)-4) above, and calculate the extraction efficiency once the extraction is stable. Extraction efficiency = Amount of phosphoric acid collected in continuous phase collection tank 11 / Amount of phosphoric acid output from self-dispersed phase feed tank 4.

[0048] In addition, the extraction clarification time of the dispersed phase in the continuous phase in the extraction chamber was also tested. The test method was as follows: continuous extraction was carried out according to the experimental steps 1)-4) above. When the extraction was stable, the introduction and discharge of the dispersed phase and the continuous phase in the extraction tower 8 were stopped, and the phases were allowed to stand and separate. It was observed that from the time of stopping, the dispersed phase in the continuous phase in the extraction chamber completely settled and formed a clear upper and lower stratification phenomenon. The time consumed was the extraction clarification time described in this application.

[0049] Following the experimental procedure described above, the extraction temperature, continuous phase flow rate, and spacing between adjacent trays in Examples 1-12, along with 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] As can be seen from Table 1, good extraction results can be achieved when the extraction temperature is 60-80℃, the extraction ratio is 1-4, and the spacing between adjacent trays is 0.8-1.2m.

[0053] Comparative Examples 1-3

[0054] According to such Figure 2 The apparatus shown was used for the extraction section of phosphoric acid purification. The experimental steps and conditions were the same as in Example 3, except that "the nozzle 7 in the extraction chamber was replaced with a feed pipe with an inner diameter of 1-3 mm and a length of 0.2 m, and the feed pipe was also arranged in the form of three vertices of an equilateral triangle". The extraction temperature was 60 °C, the continuous phase flow rate was 30 L / min, the extraction phase ratio was 4, and the tray spacing was 1 m. The experimental results are summarized in Table 2.

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

[0056] name Inner diameter of feed pipe, 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. The bottom side has an extractant feed pipe and a raffinate discharge pipe, while the top side has an extract discharge pipe. The sidewalls are equipped with 48 evenly distributed atomizing nozzles made of 316L stainless steel with a 1mm orifice diameter. The phosphoric acid to be extracted has the same composition as in Example 1. The continuous phase is a mixture of extractant and diluent. The extractant is tributyl phosphate, and the diluent is kerosene, mixed at a volume ratio of 4:1. The extraction phase ratio is 4, the tower length is 7m, and the inner diameter is 0.6m. The continuous phase solution is added to the extractant feed tank and pumped at a flow rate of 30 L / min. After passing through an extractant preheater at a temperature of 60°C, the solution enters the bottom of the extraction tower via the extractant feed pipe. The phosphoric acid to be extracted is added to the phosphoric acid feed tank and pumped at a flow rate of 7.5 L / min. It is then preheated at 60°C and atomized at nozzles on the side wall of the extraction tower, dispersing into tiny droplets that mix thoroughly with the extractant. Finally, the mixture exits from the bottom outlet of the extraction tower via a raffinate discharge pump and raffinate discharge pipe into the raffinate bottom tank. The extractant, due to its own buoyancy, moves towards the top of the extraction tower, where it comes into counter-current contact with the atomized and dispersed phosphoric acid, ultimately forming a saturated solution that exits from the top of the extraction tower into the raffinate bottom tank.

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

[0060] Comparative Example 5

[0061] According to such Figure 2The apparatus shown was used for the extraction stage of phosphoric acid purification. The experimental procedures and conditions were the same as in Example 3, except that a 5mm sieve plate was used instead of the tray with the clarification layer structure 9. The extraction temperature was 60℃, the continuous phase flow rate was 30L / min, the extraction phase ratio was 4, and the tray spacing was 1m. Ultimately, the phosphoric acid extraction efficiency was 63.6%, and the extraction clarification time was 45min.

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

Claims

1. An atomizing mixing extraction clarification device, characterized in that... The extraction tower (8) includes multiple trays inside, which divide the internal space of the extraction tower (8) into n upper and lower extraction chambers. Each extraction chamber has a dispersed phase inlet (8-3) on its upper sidewall and a dispersed phase outlet (8-4) on its lower sidewall. Along the top-to-bottom direction, nozzles (7) are provided inside the upper end of the first to the (n-1)th extraction chambers. The nozzles (7) in the extraction chambers are connected to the dispersed phase inlets (8-3) on their sidewalls through pipelines. The dispersed phase outlets (8-4) of the previous extraction chamber are connected to the dispersed phase outlets of the next adjacent extraction chambers through pipelines via dispersed phase circulation pumps (10). The inlet (8-3) allows the dispersed phase liquid at the bottom of the previous extraction chamber to be pumped into the upper end of the next adjacent extraction chamber by the dispersed phase circulation pump (10) and then atomized and dispersed into tiny droplets again by the nozzle (7). The upper 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). Each tray is provided with a tray clarification layer structure (9), and the center of the tray clarification layer structure (9) has a channel that penetrates the tray. The continuous phase of the next extraction chamber can enter the next adjacent extraction chamber through the tray clarification layer structure (9). The number of nozzles in each extraction chamber is multiple, selected from 2 to 10, and the multiple nozzles are arranged in the vertex arrangement of an equilateral triangle or the vertex arrangement of a square. The tray clarification and stratification structure (9) is an internal component of the tray, including an intermediate channel pipe (9-b) with openings at the top and bottom and a cap (9-a). The bottom or lower side wall of the intermediate channel pipe (9-b) is fixed on the tray. The cap (9-a) is fixed on the intermediate channel pipe (9-b) by a support rod. The cap (9-a) is suspended directly above the upper opening of the intermediate channel pipe (9-b). The dispersed liquid drops fall onto the cap and form a stable stratification along the cap in the outer area of ​​the intermediate channel pipe (9-b).

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

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

4. The atomizing mixing extraction clarification device as described in claim 1, characterized in that... The nozzle type is a pressure nozzle or a rotary nozzle, and the material is stainless steel, plastic or brass, with an orifice diameter of 0.1~3.0 mm.

5. The atomizing mixing extraction clarification device as described in claim 1, characterized in that... The number of nozzles in each extraction chamber is 3-5.

6. The atomizing mixing extraction clarification device as described in claim 1, characterized in that... The extraction tower (8) is equipped with a sight glass on its side. The dispersed phase inlets (8-3) of the extraction chambers other than the uppermost extraction chamber are all located close to the tower plate. The dispersed phase outlets (8-4) of the extraction chambers other than the lowermost extraction chamber are all located 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 opening of the intermediate channel fitting (9-b).

7. The process method of the atomizing mixing extraction clarification device as described in claim 1, characterized in that... Includes the following steps: 1) The continuous phase is a light phase and the dispersed phase is a heavy phase. The continuous phase is introduced from the continuous phase inlet (8-1) of the bottom extraction chamber, and enters the adjacent extraction chamber from the bottom up through the central channel of the clarified layer structure (9) of the tray, and so on, and 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 uppermost extraction chamber, atomized at the nozzle (7), and dispersed into tiny droplets. The tiny droplets of the dispersed phase settle downward and form a layer with the continuous phase in the outer area of ​​the clarified layer structure (9) of the tray. The dispersed phase layer settles on the tray and is pumped out by the dispersed phase circulation pump (10) and introduced into the upper end of the next adjacent extraction chamber. It is atomized again by the nozzle (7) and dispersed into tiny droplets. After multiple cycles, it finally enters the lowermost extraction chamber and is discharged outward from the dispersed phase outlet (8-4).

8. The process method of the atomizing mixing extraction clarification device as described in claim 7, characterized in that... The device is used in the extraction, washing, or back-extraction stages of the phosphoric acid purification process.

9. The process method of the atomizing mixing extraction clarification device as described in claim 7, characterized in that... The temperature inside the extraction tower (8) is 40~80℃, the tray spacing is 0.4~1.2 m, the dispersed phase raw material is a phosphoric acid solution with a mass fraction of 20-80%, the continuous phase includes an extractant, which is one of tributyl phosphate, methyl isobutyl ketone or isoamyl alcohol. When the extractant is selected as 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 alkanes, 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.

10. The process method of the atomizing mixing extraction clarification device as described in claim 9, characterized in that... The temperature inside the extraction tower (8) is 60-80℃, the tray spacing is 0.8-1.2m, and the volume flow ratio of the continuous phase and the dispersed phase raw materials is 2-4:1.

Citation Information

Patent Citations

  • Purified wet-process technique for producing phosphoric acid and equipment thereof

    CN1654317A

  • An improved solvent extraction process

    GB527299A