CN217613059U - Wet phosphoric acid purifying and extracting device - Google Patents
Wet phosphoric acid purifying and extracting device Download PDFInfo
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- CN217613059U CN217613059U CN202220993940.5U CN202220993940U CN217613059U CN 217613059 U CN217613059 U CN 217613059U CN 202220993940 U CN202220993940 U CN 202220993940U CN 217613059 U CN217613059 U CN 217613059U
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Abstract
The utility model relates to a wet-process phosphoric acid purification and extraction device, belonging to the technical field of wet-process phosphoric acid, wherein an aging separation chamber of the wet-process phosphoric acid purification and extraction device is in contact connection with a rotary disc tray, and the rotary disc tray is in contact connection with an aging clarification chamber; a turntable tower driving motor is arranged in the aging separation chamber and the turntable tower tray; a phosphoric acid feeding pipeline is arranged on the aging separation chamber, and a solvent feeding pipeline is arranged on the aging clarification chamber. 9-15 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-6 stages of tower plates. Feeding a phosphoric acid heavy phase and an extractant light phase according to a countercurrent contact mode; the light phase of the extractant is used as a continuous phase, the heavy phase of the phosphoric acid is used as a dispersed phase, and the phosphoric acid is dispersed into small phosphoric acid droplets through high-speed shearing when passing through a rotating disc and is fully mixed with the solvent. Phosphoric acid reacts with the solvent when mixed, and phosphoric acid molecules and solvent molecules are combined to achieve the extraction target.
Description
Technical Field
The utility model belongs to the technical field of sulfuric acid process wet process phosphoric acid purification, a purify extraction device at wet process phosphoric acid.
Background
With the rise of new energy sources and the increasing demand of phosphoric acid, the traditional phosphoric acid mainly used for producing fertilizers gradually develops towards the new energy sources, so that the purification of the phosphoric acid is particularly urgent. The traditional phosphoric acid adopts a thermal method process, is prepared by using an electric furnace method to prepare simple substance yellow phosphorus, and is oxidized and absorbed, and the obtained phosphoric acid has high purity, but has high requirements on raw materials and large energy consumption, and is not beneficial to large-scale industrial production. The wet phosphoric acid is prepared by decomposing phosphate rock with acid, separating solid and liquid to obtain phosphoric acid, and purifying to obtain pure industrial grade and food grade phosphoric acid.
The research reports about wet process phosphoric acid purification technology are many at home and abroad, the key of purification is the extraction process, the extraction method makes stirring mixing efficiency low at present, or equipment area is little but the handling capacity is not big, or because of the operation cycle length makes the mixture inhomogeneous, synthesizes above extraction characteristics, the utility model discloses a carousel tower extraction method.
The rotary disc tower type extraction can effectively solve the defects of low extraction efficiency and small extraction treatment capacity, can improve the extraction rate and reduce the spent acid half-life ratio under the condition of high impurity content of wet-process phosphoric acid, and is a new production technology which is short in technological process, small in occupied area, long in continuous operation time and suitable for large-scale production compared with other technologies.
Disclosure of Invention
So the utility model discloses a main objective provides an efficient extraction technique to the not enough of current extraction technique existence, improves the extraction rate and reduces raffinate acid yield, reduction in production cost.
In order to achieve the above purpose, the utility model adopts the technical scheme that:
the aging separation chamber of the wet-process phosphoric acid purification extraction device is in contact connection with a turntable tray, and the turntable tray is in contact connection with an aging clarification chamber; a turntable tower driving motor is arranged in the aging separation chamber and the turntable tower tray;
the aging separation chamber is provided with a phosphoric acid feeding pipeline, and the aging clarification chamber is provided with a solvent feeding pipeline.
9-15 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-6 stages of tower plates.
As a preferred scheme, 9 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-4 stages of tower plates;
and 10 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-4 stages of tower plates.
11 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-4 stages of tower plates.
12 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-5 stages of tower plates.
13 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-5 stages of tower plates.
And 14 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between the 1-5 stages of tower plates.
15 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-6 stages of tower plates.
16 stages of tower plates are arranged in the turntable tower tray, and extraction sampling detection points are arranged between 1-6 stages of tower plates.
After the number of the tower plates is increased to be more than 18 grades, the raffinate acid has poor flowability due to serious enrichment of raffinate acid impurities, so that the subsequent desorption treatment of the raffinate acid is not facilitated, and the preferred grade is 10.
The aperture of each stage of tower plate is 10-20mm, and the middle of each two stages of tower plates is provided with 4-6 radial blades for providing the thrust of the radial flow of the fluid.
An extraction solvent discharging pipeline is arranged on the aging separation chamber, and an extraction product monitoring point is arranged on the pipeline; the aging and clarifying chamber is provided with a raffinate acid discharging pipeline which is provided with a discharging content monitoring point.
A wet-process phosphoric acid purification extraction method comprises the following steps:
(1) Pumping wet phosphoric acid into an aging separation chamber, and pumping an extracting agent into an aging clarification chamber;
(2) Phosphoric acid as a disperse phase enters a turntable tray from the aging separation chamber downwards, an extracting agent as a continuous phase enters the turntable tray from the aging clarification chamber, the phosphoric acid and the extracting agent are contacted in a countercurrent contact mode in the turntable tray, and are sheared, dispersed and mixed on a turntable for extraction, so that purified phosphoric acid is obtained.
The wet-process phosphoric acid phosphorus pentoxide mass fraction is 52.5% -54.0%, the sulfate radical mass fraction is 0.2% -0.4%, and the iron ion mass fraction is 0.159% -0.25%.
The extracting agent comprises methyl isobutyl ketone, n-butyl alcohol, tributyl phosphate and a composite extracting agent of the methyl isobutyl ketone and the n-butyl alcohol or the tributyl phosphate, and the flow rate of the extracting agent entering the aging clarifying chamber is 60-70kg/h.
Wet phosphoric acid and extractant enter the turntable tray and the phase ratio is controlled to be 3.5-5.5 (mass ratio).
Before the wet-process phosphoric acid is pumped into the aging separation chamber, the tray of the rotary disc tower is filled with the extracting agent, and a driving motor of the rotary disc tower is started to stir, wherein the stirring speed is controlled to be 500-660rpm, such as 510rpm, 550rpm, 580rpm, 600rpm and 660 rpm. In the scheme, the reaction temperature is 20-45 ℃.
The rotating speed plays an important role in the dispersion and contact of two phases, when the rotating speed is lower than 400rpm, the heavy phase dispersion is poor, the extraction efficiency is low, and the extraction spent acid yield is high; when the rotating speed is too high, for example, above 680rpm, the heavy phase is dispersed into very small droplets, the continuous flow of the light phase is interrupted, the emulsification phenomenon is easy to occur, and the entrainment of the light phase is serious.
The device is adopted to carry out the wet-process phosphoric acid purification extraction process, as a preferred scheme, 10 stages of tower plates are arranged in the turntable tower tray, the aperture of each stage of tower plate is 10-20mm, and 4-6 radial blades are arranged between every two layers of tower plates to provide the thrust for the radial flow of fluid.
The extractant after extraction overflows to the next process from the top of the aging separation chamber, the unextracted phosphoric acid enters a raffinate acid system from the bottom of the aging clarification chamber, the mass conservation relation is formed among the flow of the ortho-acid, the flow of the no-load solvent, the flow of the load solvent and the flow of the raffinate acid, generally, the ratio of the ortho-acid to the raffinate acid is controlled to be 2-2.6, and the closer to 2.6, the higher the extraction rate is. Too high, the concentration of raffinate acid impurities is serious, the continuity of the device is poor, and the production is not facilitated. The closer to 2, the higher the raffinate acid yield, the lower the extraction efficiency, and the lower the extraction efficiency, the higher the raffinate acid yield, and the lower the device efficiency.
The technical scheme of the utility model in, light phase solvent gets into the carousel tower from the tower bottom by light phase solvent charge-in line and is full of whole tower, heavy phase phosphoric acid gets into the carousel tower from the top of the tower by heavy phase phosphoric acid charge-in line, heavy phase relies on self action of gravity to subside in-process and ascending light phase solvent contact tray, the tray is driven by driving motor and is done the shearing motion, the material is because the high-speed dispersion of shearing operation takes place extraction reaction on the tray, dispersed material continues to descend to next tray after the reunion again, it takes place extraction reaction to be dispersed again by the mixture again, therefore light phase is continuous by the dispersion extraction reaction at the ascending in-process, the phosphoric acid content in the light phase risees gradually, heavy phase descends in-process phosphoric acid content gradually, final light phase is got rid of from top of the tower extraction solvent ejection of compact line 7, heavy phase raffinate spent acid gets rid of from bottom raffinate spent acid ejection of compact line, the rectification process is carried out the sample check analysis to business turn over material and is convenient for adjusting motor speed.
Adopt the technical scheme of the utility model following beneficial effect does have:
(1) The utility model has high mass transfer efficiency, the mass fraction of phosphorus pentoxide in the raffinate is 34-36%, and the extraction rate reaches more than 65%.
(2) The utility model discloses the device is simple, and area is little, and the extraction process is convenient for control, easily industrialization implementation.
Drawings
FIG. 1 is a diagram of a wet-process phosphoric acid purification and extraction apparatus, wherein 1-a rotating disc tower driving motor, 2-an aging separation chamber, 3-an aging clarification chamber, 4-a rotating disc tower tray, 5-a phosphoric acid feeding pipeline, 6-a solvent feeding pipeline, 7-an extraction solvent discharging pipeline, 8-a raffinate acid discharging pipeline, 9-a discharging content monitoring point, 10-an extraction sampling detection point and 11-an extraction product monitoring point.
Fig. 2 is a rotating tray configuration with 12 fixed trays, 13 radial vanes, 14 tray mesh, and 15 impeller shafts.
Detailed Description
For a better understanding of the present invention, the following examples are provided to further illustrate the present invention, but the present invention is not limited to the following examples.
Example 1
In the wet-process phosphoric acid purification and extraction device, an aging separation chamber 2 is in contact connection with a turntable tower tray 4, and the turntable tower tray 4 is in contact connection with an aging clarification chamber 3; a turntable tower driving motor 1 is arranged in the aging separation chamber 2 and the turntable tower tray 4; a phosphoric acid feeding pipeline 5 is arranged on the aging separation chamber 2, and a solvent feeding pipeline 6 is arranged on the aging clarification chamber 3. 10-stage tower plates are arranged in the turntable tower tray 4, and extraction sampling detection points 10 are arranged between the 1-4-stage tower plates.
Each stage of tower plate consists of 2 layers of fixed tower plates 12, tower plate sieve holes 14 are arranged on the fixed tower plates 12, the aperture of each stage of tower plate is 13mm, and 4 radial blades 13 are arranged in the middle of every two layers of tower plates and are fixed in the middle of the turntable tower plate 4 through an impeller shaft 15 for providing fluid radial flow thrust. An extraction solvent discharging pipeline 7 is arranged on the aging separation chamber 2, and an extraction product monitoring point 11 is arranged on the pipeline; an extraction spent acid discharging pipeline 8 is arranged on the aging and clarifying chamber 3, and a discharging content monitoring point 9 is arranged on the pipeline.
Example 2
The extraction process of wet-process phosphoric acid by using the apparatus of example 1 includes the following specific processes:
in the wet-process phosphoric acid purification and extraction process designed in this example, the composition table of the wet-process phosphoric acid is shown in table 1 below
TABLE 1 ingredient Table of wet process phosphoric acid
| Composition (I) | P 2 O 5 | SO 4 2- | Fe |
| Content/%) | 53.43 | 0.22 | 0.1978 |
| Specific gravity/kg/ | 1.757 |
(1) The rotating disc tower is filled with an extractant MIBK, a driving motor of the rotating disc tower is started to stir, the stirring speed is controlled to be 510rpm, and the temperature in the rotating disc tower is controlled to be 35 ℃;
(2) Pumping wet-process phosphoric acid into an aging separation chamber, and pumping an extracting agent MIBK and phosphoric acid into an aging clarification chamber according to a mass ratio of 5;
(3) Phosphoric acid as a disperse phase enters a rotating disc tray from an aging separation chamber downwards, an extracting agent as a continuous phase enters the rotating disc tray from an aging clarification chamber, the phosphoric acid and the extracting agent are contacted in a countercurrent contact mode in the rotating disc tray and are sheared, dispersed and mixed on a rotating disc for extraction, the extracted extracting agent overflows from the upper part of the aging separation chamber, and raffinate and raffinate are discharged from the bottom of the tower to obtain purified phosphoric acid-1.
The apparatus of example 1 was further subjected to 8-stage, 12-stage, 16-stage, 18-stage plate numbers and two-stage emulsification under the process conditions of this example, to obtain phosphoric acid-2, phosphoric acid-3, phosphoric acid-4, phosphoric acid-5, and phosphoric acid-6. The effect is as follows:
remarking: in which P is involved 2 O 5 The extraction rate was calculated as: extraction rate = (P of raw material acid) 2 O 5 content-P in raffinate 2 O 5 Content) with P of the starting acid 2 O 5 And (4) content.
The bipolar emulsification step is that the impeller of the emulsification pump is used for shearing and mixing, and the materials are mixed and extracted by adopting two-stage countercurrent contact.
Claims (4)
1. The wet-process phosphoric acid purification and extraction device is characterized in that an aging separation chamber (2) is in contact connection with a turntable tray (4), and the turntable tray (4) is in contact connection with an aging clarification chamber (3);
a turntable tower driving motor (1) is arranged inside the aging separation chamber (2) and the turntable tower tray (4);
a phosphoric acid feeding pipeline (5) is arranged on the aging separation chamber (2), and a solvent feeding pipeline (6) is arranged on the aging clarification chamber (3).
2. The purification and extraction device for the wet-process phosphoric acid according to claim 1, wherein 9-15 stages of tower plates are arranged in the turntable tray (4), and extraction sampling detection points (10) are arranged between 1-6 stages of tower plates.
3. The purification and extraction device for wet-process phosphoric acid according to claim 2, characterized in that each stage of the trays consists of 2 fixed trays (12), the fixed trays (12) are provided with tray sieve holes (14),
the aperture of the tower plate sieve hole (14) is 10-20mm, and 4-6 radial blades (13) are arranged in the middle of each two layers of tower plates and are fixed in the middle of the turntable tower plate (4) through an impeller shaft (15).
4. The purification and extraction device for wet-process phosphoric acid according to claim 1, characterized in that the aging separation chamber (2) is provided with an extraction solvent discharge line (7) which is provided with an extraction product monitoring point (11);
an extraction spent acid discharging pipeline (8) is arranged on the aging and clarifying chamber (3), and a discharging content monitoring point (9) is arranged on the pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220993940.5U CN217613059U (en) | 2022-04-27 | 2022-04-27 | Wet phosphoric acid purifying and extracting device |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220993940.5U CN217613059U (en) | 2022-04-27 | 2022-04-27 | Wet phosphoric acid purifying and extracting device |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653095A (en) * | 2022-04-27 | 2022-06-24 | 宜都兴发化工有限公司 | Wet-process phosphoric acid purification and extraction device and method |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114653095A (en) * | 2022-04-27 | 2022-06-24 | 宜都兴发化工有限公司 | Wet-process phosphoric acid purification and extraction device and method |
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