CN219290639U - Device for extracting organic solvent from raffinate acid in phosphoric acid production by wet purification - Google Patents
Device for extracting organic solvent from raffinate acid in phosphoric acid production by wet purification Download PDFInfo
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- CN219290639U CN219290639U CN202320361053.0U CN202320361053U CN219290639U CN 219290639 U CN219290639 U CN 219290639U CN 202320361053 U CN202320361053 U CN 202320361053U CN 219290639 U CN219290639 U CN 219290639U
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- 239000002253 acid Substances 0.000 title claims abstract description 113
- NBIIXXVUZAFLBC-UHFFFAOYSA-N Phosphoric acid Chemical compound OP(O)(O)=O NBIIXXVUZAFLBC-UHFFFAOYSA-N 0.000 title claims abstract description 38
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 22
- 229910000147 aluminium phosphate Inorganic materials 0.000 title claims abstract description 19
- 239000003960 organic solvent Substances 0.000 title claims abstract description 16
- 238000000746 purification Methods 0.000 title claims abstract description 14
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 24
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 18
- 239000010439 graphite Substances 0.000 claims abstract description 18
- 238000004140 cleaning Methods 0.000 claims abstract description 14
- 239000000945 filler Substances 0.000 claims abstract description 14
- 239000002699 waste material Substances 0.000 claims abstract description 9
- 239000007921 spray Substances 0.000 claims abstract description 5
- 239000007788 liquid Substances 0.000 claims description 13
- 238000012856 packing Methods 0.000 claims description 7
- 238000012546 transfer Methods 0.000 claims description 5
- 238000003860 storage Methods 0.000 claims description 3
- 238000003795 desorption Methods 0.000 abstract description 5
- 239000012530 fluid Substances 0.000 abstract 1
- 239000002904 solvent Substances 0.000 description 13
- 238000000034 method Methods 0.000 description 9
- 239000000047 product Substances 0.000 description 8
- 239000000463 material Substances 0.000 description 7
- 229910052799 carbon Inorganic materials 0.000 description 6
- 239000003337 fertilizer Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 4
- 230000007797 corrosion Effects 0.000 description 3
- 238000005260 corrosion Methods 0.000 description 3
- 238000011049 filling Methods 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000004821 distillation Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000011148 porous material Substances 0.000 description 2
- 230000002035 prolonged effect Effects 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910000963 austenitic stainless steel Inorganic materials 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000008901 benefit Effects 0.000 description 1
- 230000000903 blocking effect Effects 0.000 description 1
- 239000006227 byproduct Substances 0.000 description 1
- 239000012459 cleaning agent Substances 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 229910001039 duplex stainless steel Inorganic materials 0.000 description 1
- 238000000605 extraction Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 229910000040 hydrogen fluoride Inorganic materials 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000002912 waste gas Substances 0.000 description 1
- 238000009736 wetting Methods 0.000 description 1
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P20/00—Technologies relating to chemical industry
- Y02P20/10—Process efficiency
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- Devices And Processes Conducted In The Presence Of Fluids And Solid Particles (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
The device for removing the organic solvent from the raffinate acid in the phosphoric acid production by wet purification comprises an equipment main body, a circulating axial flow pump, a graphite heater, a raffinate acid feeding pump and a demister; the equipment main body is of a vertical cylinder structure, and a secondary tank acid distributor, a tetrafluoro spray head, grid fillers and a grid supporting ring are fixedly arranged in the equipment main body; the upper part of the equipment main body is provided with a waste steam outlet, a raffinate inlet and a cleaning fluid inlet, and the lower part is provided with a circulating acid inlet, a circulating acid outlet, a pressure measuring hole and an overflow port; the demister is connected with a waste steam outlet through a pipeline, the inlet of the circulating axial flow pump is connected with a circulating acid outlet through a pipeline, the outlet of the circulating axial flow pump is connected with a graphite heater inlet through a pipeline, the outlet of the graphite heater is connected with a circulating acid inlet through a pipeline, and the raffinate acid feed pump is connected with a raffinate acid inlet through a pipeline. The utility model has good anti-blocking performance, reduces the cleaning workload, reduces the stopping time caused by equipment blockage, and solves the problem that the traditional raffinate acid concentration desorption tower is difficult to clean.
Description
Technical Field
The utility model belongs to the technical field of wet-process phosphoric acid purification production, and particularly relates to a device for removing organic solvent from raffinate acid in wet-process phosphoric acid purification production.
Background
The wet phosphoric acid purification uses an organic solvent as an extractant, and a byproduct after the phosphoric acid purification is extracted to be raffinate acid, wherein the raffinate acid contains 0.05% -0.25% of the extractant (calculated by total organic carbon TOC). The raffinate acid contains solid matters, the solid content of the raffinate acid before concentration and desorption is 1% -2%, the impurity concentration is increased in the concentration process, more precipitate is separated out, the strength of the precipitate is hard, the acid-resistant cleaning liquid is corroded, the common cleaning agent in the phosphoric acid concentration industry can not be cleaned, and the precipitate blocks the tower body after about 7 days, so that the tower body is forced to stop.
Raffinate phosphoric acid is generally used as a fertilizer for the removal of organic solvents due to: 1) Recovering the solvent and reducing the solvent consumption; 2) The solvent has large smell, is easy to accumulate in low-lying places, is inflammable, and increases the danger of the operation environment; 3) Ensures the use safety of the fertilizer, and the fertilizer is stored, transported and has no volatile organic solvent in use.
At present, the generally used extraction residual acid concentration desorption towers in China are plate type rectifying towers and common concentration distillation towers. The operation temperature of the plate type rectifying tower is 85 ℃, the operation pressure is-20 kpa, and the Total Organic Carbon (TOC) content of the product is less than 0.015%. The plate type rectifying tower has low requirements on equipment materials, but the mounting requirements on bubble caps of the tower plate accessory are extremely high, about 500-2000 bubble caps of each raffinate acid desorber are unequal, the bubble caps are easy to scale, the cleaning workload is large, and the influence on production is extremely large. The common concentration distillation tower has the operating temperature of 105-110 ℃ and the operating pressure of-45 kpa, has extremely high corrosion resistance requirement on equipment materials, has high steam consumption, has the Total Organic Carbon (TOC) content of less than 0.02 percent, has high total organic carbon content, and is eliminated gradually.
Disclosure of Invention
The utility model aims to solve the defects of the prior art and provides a device for removing organic solvent by adding raffinate acid in the production of wet-process purified phosphoric acid. The large-aperture grid filler is used in the raffinate acid concentration desorption tower and used for wet phosphoric acid purification production, the equipment structure is simple, the filler anti-blocking performance is good, the cleaning workload is reduced, the stopping time caused by equipment blocking is shortened, the problem that the traditional raffinate acid concentration desorption tower is difficult to clean is solved, and the production cost is reduced.
In order to achieve the above object, the present utility model provides the following technical solutions: the device for removing the organic solvent from the raffinate acid in the phosphoric acid production by wet purification comprises an equipment main body, a circulating axial flow pump, a graphite heater, a raffinate acid feeding pump and a demister; wherein,,
the equipment main body is of a vertical cylinder structure, the upper part of the equipment main body is provided with an elliptical end socket, and the lower part of the equipment main body is of a cone structure; a secondary groove type acid distributor, a tetrafluoro spray head, grid filler and a grid supporting ring are sequentially and fixedly arranged in the equipment main body from top to bottom, and the grid filler is arranged on the grid supporting ring; the upper part of the equipment main body is provided with a waste steam outlet, a raffinate inlet and a cleaning liquid inlet; the raffinate acid inlet is connected with a secondary groove type acid separator; the lower part of the equipment main body is provided with a circulating acid inlet, a circulating acid outlet, a pressure measuring hole and an overflow port; the equipment main body is also provided with a plurality of manholes;
the steam inlet of the demister is connected with the waste steam outlet through a pipeline, the steam outlet of the demister is connected with the vacuum pump air inlet through a pipeline, the circulating axial flow pump inlet is connected with the circulating acid outlet through a pipeline, the circulating axial flow pump outlet is connected with the graphite heater inlet through a pipeline, the graphite heater outlet is connected with the circulating acid inlet through a pipeline, the raffinate acid feed pump outlet is connected with the raffinate acid inlet through a pipeline, and the raffinate acid feed pump inlet is connected with the raffinate acid transfer storage tank through a pipeline.
Preferably, the apparatus further comprises a return acid pump; the inlet of the return acid pump is connected to a pipeline connecting the circulating axial flow pump with the graphite heater; the outlet of the return acid pump is connected to a conduit connecting the raffinate feed pump with the raffinate inlet.
Preferably, the lower part of the equipment main body is also provided with a double-flange liquid level meter, and the double-flange liquid level meter is connected with the equipment main body through a hole site A and a hole site B which are arranged on the equipment main body.
Preferably, the grid packing is divided into 4-8 sections.
Preferably, the grid packing is rectangular and square, and the diameter of the holes is 120mm or 120mm.
The utility model has the beneficial effects that:
(1) According to the utility model, the large open-pore grid packing tower is used for concentrating raffinate acid and removing organic solvent in wet phosphoric acid purification production, and production practice proves that the tower has good anti-blocking performance, the shutdown cleaning time is prolonged from 7 days to 6 months, the cleaning workload is reduced, and the problem that the scaling of the traditional raffinate acid concentration tower is extremely difficult to clean is solved;
(2) The Total Organic Carbon (TOC) content of the product is lower than that of the traditional process, and is less than 0.01%, so that the efficiency of removing organic matters is improved, and the application channel of raffinate acid is widened;
(3) The corrosion resistance requirement on equipment materials is low, and the investment is low;
(4) The safety of the terminal product is improved, and the production environment is good for fertilizer production and manufacturing;
(5) The manufacturing and the installation of the internal structural parts of the equipment are simple;
(6) The extractant is expensive, more extractant is recovered, and the economic benefit is higher.
Drawings
FIG. 1 is a schematic diagram of the present utility model.
Description of the embodiments
Embodiments of the present utility model will now be described with reference to the accompanying drawings, and it will be understood by those skilled in the art that the following examples are for illustration only and should not be construed as limiting the scope of the utility model. The specific techniques, connections, or conditions are not identified in the examples and are set forth in accordance with the techniques, connections, conditions, or in accordance with the product specifications described in the literature in this field. The materials, instruments or equipment used are conventional products available from commercial sources, not identified to the manufacturer.
In the description of the present utility model, it should be noted that, unless explicitly stated and limited otherwise, the terms "mounted," "connected," and "provided" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium. The specific meaning of the above terms in the present utility model is understood by those of ordinary skill in the art according to the specific circumstances.
As shown in fig. 1, the device for removing the organic solvent from the raffinate acid in the phosphoric acid production by wet purification provided by the utility model comprises an equipment main body 1, a circulating axial flow pump 7, a graphite heater 11, a raffinate acid feed pump 12 and a demister 14; wherein,,
the equipment main body 1 (tower body) is of a vertical cylinder structure, the upper part of the equipment main body is provided with an elliptical seal head 17, and the lower part of the equipment main body is provided with a cone 18 structure; the material of the equipment main body 1 is super duplex stainless steel 2507 or super austenitic stainless steel 904L, so as to prevent the corrosion of hydrogen fluoride in raffinate acid; a secondary groove type acid distributor 19, a tetrafluoro spray head 20, a grid filler 21 and a grid support ring 22 are sequentially and fixedly arranged in the equipment main body 1 from top to bottom, and the grid filler 21 is arranged on the grid support ring 22; the tetrafluoro spray head 20 can clean the filler in an out-of-stop state; the grid support ring 22 can prevent the filler from moving due to steam impact; the grid packing 21 is divided into 4-8 sections; the grid filler 21 is rectangular square, the diameter of holes is 120mm or 120mm, the large-opening grid filler has good anti-blocking performance, and the cleaning period is prolonged; the upper part of the equipment main body 1 is provided with a waste steam outlet 6, a raffinate acid inlet 15 and a cleaning liquid inlet 2, wherein the waste steam outlet 6 is arranged at the top of an elliptical seal head 17, the height of the raffinate acid inlet 15 is higher than that of the cleaning liquid inlet 2, and the raffinate acid inlet 15 and the cleaning liquid inlet 2 are respectively positioned at two sides of the equipment main body 1; the raffinate acid inlet 15 is connected with a secondary tank acid distributor 19, and the purpose of adopting the secondary tank acid distributor is to uniformly disperse raffinate acid into small liquid drops so as to increase the heat and mass transfer effect; the lower part of the equipment main body 1 is provided with a circulating acid inlet 23, a circulating acid outlet 24, a pressure measuring hole 16 and an overflow port 5, wherein the circulating acid outlet 24 is positioned at the lowest part of the equipment main body 1, the height of the overflow port 5 is higher than that of the circulating acid inlet 23, the circulating acid inlet 23 and the circulating acid inlet 5 are respectively positioned at two sides of the equipment main body 1, and the pressure measuring hole 16 is positioned above the overflow port 5; by arranging the pressure measuring holes 16, the pressure drop condition of the packed tower can be observed at any time, and whether the tower needs to be shut down or not can be judged on line; the equipment main body 1 is also provided with a plurality of manholes 3;
the steam inlet of the demister 14 is connected with the waste steam outlet 6 through a pipeline, and the steam outlet of the demister 14 is connected with the air inlet of the vacuum pump 29 through a pipeline, so as to collect raffinate drops entrained in waste gas and reduce product loss; the inlet of the circulating axial flow pump 7 is connected with the circulating acid outlet 24 through a pipeline, the outlet of the circulating axial flow pump 7 is connected with the inlet of the graphite heater 11 through a pipeline, the outlet of the graphite heater 11 is connected with the circulating acid inlet 23 through a pipeline, the outlet of the raffinate acid feeding pump 12 is connected with the raffinate acid inlet 15 through a pipeline, and the inlet of the raffinate acid feeding pump 12 is connected with the raffinate acid transfer storage tank 13 through a pipeline. The temperature difference of the circulating acid at the inlet and outlet of the solvent-resistant graphite heater is preferably 3-5 ℃, and the aim is to prevent the heat exchange tube from breaking due to thermal expansion exceeding the bearing capacity of the heat exchange tube.
Further optimizing scheme, the device also comprises a return acid pump 8 for taking part of acid from the circulation pipeline and returning the acid to the main body 1 of the equipment; the inlet of the return acid pump 8 is connected to a pipe connecting the circulation axial flow pump 7 with the graphite heater 11; the outlet of the return acid pump 8 is connected to a pipeline connecting the raffinate acid feeding pump 12 and the raffinate acid inlet 15, specifically through a tee joint, and a valve is arranged at each of three ports of the tee joint for controlling the flow direction of materials; a valve is also arranged on the pipeline at the inlet of the return acid pump 8; the flow rate of the returned acid is required to meet the acid spraying density of more than 8m 3 /m 2 H, and the volume ratio of the return acid to the initial raffinate is 2:1, with the aim of fully wetting the packing; the volume ratio of the recycle acid to the mixed acid at the raffinate acid inlet 15 is 120-150:1, and the aim is to increase the temperature of the tower kettle and further reduce the total organic carbon content in the product.
Further optimizing scheme still is equipped with two flange level gauges in equipment main part 1 lower part, and two flange level gauges are connected with equipment main part 1 through hole site A4a and hole site B4B that set up on the equipment main part 1.
The working principle of the utility model is as follows: the large open pore grating filler has the effect of increasing the contact area of vapor and liquid phases in the tower, the raffinate acid containing the solvent enters the tower from the top of the tower, the raffinate acid flows to the tower kettle under the action of gravity, the raffinate acid in the circulating pipeline exchanges heat with the solvent-resistant graphite heat exchanger, the temperature of the raffinate acid is increased, the moisture is evaporated to become water vapor which flows upwards, and the water vapor and the raffinate acid flowing downwards generate a heat and mass transfer process. The solvent belongs to substances with relatively high probability, the raffinate acid belongs to substances with relatively low volatility, the upper part of the whole tower belongs to a stripping section, the lower part of the whole tower belongs to a rectifying section, the solvent content in the stripping section is gradually reduced from bottom to top, the solvent content at the top of the tower is minimum, the solvent content in the rectifying section is gradually increased from top to bottom, and the solvent content in the tower bottom is highest. According to the principle of rectification, the solvent gradually decreases from bottom to top in the tower, thereby achieving the purpose of reducing the solvent content in the raffinate acid.
The operation process of the utility model is as follows:
step one, tower filling: closing an outlet valve A25 of the return acid pump 8, opening a valve B26 and a valve C27, starting the raffinate feed pump 12, filling raffinate into the tower, and observing the numerical value of the double-flange liquid level meter; starting a heating device: introducing steam into the graphite heater 11, allowing the steam to enter through the inlet 10, performing heat exchange, condensing into steam condensate water, and discharging from the outlet 9; and thirdly, starting a return acid pump 8: opening a valve A25 and a valve D28, starting a return acid pump 8 to inject a mixture of the raffinate acid and the return acid into the tower, wherein the volume ratio of the return acid to the initial raffinate acid is 2:1; starting a circulating axial flow pump: starting a circulating axial flow pump 7, and controlling the volume ratio of the circulating acid to the mixed acid of the raffinate acid inlet 15 to be 120-150:1; and fifthly, starting a vacuum pump 29, controlling the pressure in the tower to be-20 KPa, controlling the temperature to be 85 ℃, and after the tower is stably operated for a period of time, extracting qualified product acid from an overflow port 5 of the tower kettle. During operation, the pressure measuring hole 16 is observed, pure water is sprayed from the cleaning liquid inlet 2 when the pressure is reduced, and the filling material is washed, so that the pressure is recovered to be normal.
The above embodiments are only illustrative of the preferred embodiments of the present utility model and are not intended to limit the scope of the present utility model, and various modifications and improvements made by those skilled in the art to the technical solutions of the present utility model should fall within the protection scope defined by the claims of the present utility model without departing from the design spirit of the present utility model.
Claims (5)
1. The device for removing the organic solvent from the raffinate acid in the phosphoric acid production by wet purification is characterized by comprising an equipment main body (1), a circulating axial flow pump (7), a graphite heater (11), a raffinate acid feed pump (12) and a demister (14); wherein,,
the equipment main body (1) is of a vertical cylinder structure, an elliptical end socket (17) is arranged at the upper part of the equipment main body, and a cone (18) structure is arranged at the lower part of the equipment main body; a secondary groove type acid distributor (19), a tetrafluoro spray head (20), a grid filler (21) and a grid support ring (22) are sequentially and fixedly arranged in the equipment main body (1) from top to bottom, and the grid filler (21) is arranged on the grid support ring (22); the upper part of the equipment main body (1) is provided with a waste steam outlet (6), a raffinate inlet (15) and a cleaning liquid inlet (2); the raffinate inlet (15) is connected with a secondary groove type acid separator (19); the lower part of the equipment main body (1) is provided with a circulating acid inlet (23), a circulating acid outlet (24), a pressure measuring hole (16) and an overflow port (5); a plurality of manholes (3) are also arranged on the equipment main body (1);
the steam inlet of the demister (14) is connected with the waste steam outlet (6) through a pipeline, the steam outlet of the demister (14) is connected with the air inlet of the vacuum pump (29) through a pipeline, the inlet of the circulating axial flow pump (7) is connected with the circulating acid outlet (24) through a pipeline, the outlet of the circulating axial flow pump (7) is connected with the inlet of the graphite heater (11) through a pipeline, the outlet of the graphite heater (11) is connected with the circulating acid inlet (23) through a pipeline, the outlet of the raffinate feed pump (12) is connected with the raffinate inlet (15) through a pipeline, and the inlet of the raffinate feed pump (12) is connected with the raffinate transfer storage tank (13) through a pipeline.
2. The apparatus for stripping organic solvent from raffinate acid in wet clean phosphoric acid production according to claim 1, characterized in that the apparatus further comprises a return acid pump (8); the inlet of the return acid pump (8) is connected to a pipeline connecting the circulating axial flow pump (7) with the graphite heater (11); the outlet of the return acid pump (8) is connected to a conduit connecting the raffinate feed pump (12) with the raffinate inlet (15).
3. The device for removing the organic solvent from the raffinate acid in the phosphoric acid wet purification production according to claim 1, wherein a double-flange liquid level meter is further arranged at the lower part of the equipment main body (1), and the double-flange liquid level meter is connected with the equipment main body (1) through a hole site A (4 a) and a hole site B (4B) arranged on the equipment main body (1).
4. Device for stripping organic solvent from raffinate acid in the production of wet purified phosphoric acid according to claim 1, characterized in that the grid packing (21) is divided into 4-8 sections.
5. The device for stripping organic solvent from raffinate acid in phosphoric acid production by wet purification according to claim 1 or 4, wherein the grid packing (21) is rectangular square lattice, and the diameter of the holes is 120mm by 120mm.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320361053.0U CN219290639U (en) | 2023-03-02 | 2023-03-02 | Device for extracting organic solvent from raffinate acid in phosphoric acid production by wet purification |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202320361053.0U CN219290639U (en) | 2023-03-02 | 2023-03-02 | Device for extracting organic solvent from raffinate acid in phosphoric acid production by wet purification |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN219290639U true CN219290639U (en) | 2023-07-04 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202320361053.0U Active CN219290639U (en) | 2023-03-02 | 2023-03-02 | Device for extracting organic solvent from raffinate acid in phosphoric acid production by wet purification |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN219290639U (en) |
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2023
- 2023-03-02 CN CN202320361053.0U patent/CN219290639U/en active Active
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