CN216825200U - Separation and purification system for fluosilicic acid and silicon dioxide mixed slurry - Google Patents
Separation and purification system for fluosilicic acid and silicon dioxide mixed slurry Download PDFInfo
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- CN216825200U CN216825200U CN202220400424.7U CN202220400424U CN216825200U CN 216825200 U CN216825200 U CN 216825200U CN 202220400424 U CN202220400424 U CN 202220400424U CN 216825200 U CN216825200 U CN 216825200U
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Abstract
The utility model provides a separation and purification system for fluosilicic acid and silica mixed slurry. The device comprises a solid-liquid separator and an input unit, wherein the solid-liquid separator is used for separating fluosilicic acid from silicon dioxide; the steam input unit is used for conveying steam into the solid-liquid separator to purify the silicon dioxide; the washing liquid input unit is used for conveying washing liquid into the solid-liquid separator to wash the silicon dioxide; and the mixed slurry input unit is used for conveying the fluosilicic acid and the silicon dioxide into the solid-liquid separator. The utility model greatly reduces the fluorine content of the fluorine-containing silicon slag and improves the purity and the specific surface area of the product; low production cost, reduced solid waste discharge, environmental protection and suitability for large-scale popularization.
Description
Technical Field
The utility model relates to an inorganic acid and silica separation and purification technical field especially relate to a separation and purification system that is used for fluosilicic acid and mixed ground paste of silica.
Background
In the production process of phosphoric acid and hydrogen fluoride, a mixed slurry of fluosilicic acid and silicon dioxide is produced as a byproduct. The product is from phosphate ore (3 Ca)3(PO4)2CaF2) In the process for producing phosphoric acid, fluorine in the phosphoric acid mostly escapes in the form of silicon tetrafluoride gas, and the mixed slurry of fluosilicic acid and silicon dioxide is generated in a water washing absorption mode, because the chemical bond energies of fluorine ions and hydroxyl ions are close, the reaction of the silicon tetrafluoride gas and water in an acidic environment is a stepwise reversible reaction, and the reaction mechanism is as follows:
the overall reaction chemical equation:
the generated hydrogen fluoride continuously carries out reversible reaction with the silicon tetrafluoride to generate fluosilicic acid:
therefore, the mixture of fluosilicic acid and silica slurry has complex ion state, the silica solid has porosity and strong adsorption capacity, a large amount of free fluorine ions are adsorbed on the surface of the silica generated by reaction in the production process, and the cavity formed in the amorphous structure of the silica contains a large amount of fluorine elements with complex ion state and is difficult to separate. The fluorine is mainly present in the form of free fluorine and lattice fluorine. The free fluorine, which is about 70%, is mainly fluorosilicic acid adhered to the surface of silica, and can be removed by rinsing. About 30% of lattice fluorine is caused by the crystal defects generated when fluorine in the solution occupies the oxygen element site during the crystallization of silica. Since lattice fluorine forms a chemical bond with silicon atoms, physical washing cannot remove it. Therefore, the silicon dioxide contains a certain amount of fluorine which is harmful to the environment, and the direct discharge not only pollutes the environment, but also is a waste of resources. With the development of phosphate fertilizer industry in China, the amount of fluorine-containing silicon slag is increased more and more, and the utilization of the byproduct fluorine-containing silicon slag becomes a problem to be solved urgently in the phosphate fertilizer industry.
In the existing device, the steps for separating and purifying the silicon dioxide are as follows: and performing solid-liquid separation on the silicon dioxide by using a traditional plate and frame filter to obtain a fluorosilicic acid solution and silicon dioxide filter residues, and then calcining the silicon dioxide filter residues at high temperature to remove fluorine elements and purifying the silicon dioxide. However, the device can destroy the microstructure of the silicon dioxide due to higher heating temperature, reduce the oil absorption value and the specific surface area, seriously affect the performance of the silicon dioxide and reduce the utilization value of the silicon dioxide.
SUMMERY OF THE UTILITY MODEL
To exist not enough among the prior art, the utility model provides a separation and purification system for fluosilicic acid and mixed ground paste of silica, it has solved the performance that exists silica among the prior art and has reduced, problem that the use value is not high.
A separation and purification system for fluosilicic acid and silicon dioxide mixed slurry comprises a solid-liquid separator and an input unit, wherein the solid-liquid separator is used for separating fluosilicic acid and silicon dioxide, the input end of the solid-liquid separator is communicated with the input unit,
the input unit comprises a water vapor input unit, a washing liquid input unit and a mixed slurry input unit;
the steam input unit is used for conveying steam into the solid-liquid separator to purify the silicon dioxide;
the washing liquid input unit is used for conveying washing liquid into the solid-liquid separator to wash the silicon dioxide;
and the mixed slurry input unit is used for conveying the fluosilicic acid and the silicon dioxide into the solid-liquid separator.
Further, the input unit also comprises a hot air input unit which is communicated with the solid-liquid separator through a hot air input pipe and is used for conveying hot air into the solid-liquid separator to dry the silicon dioxide.
Further, the hot air input unit comprises an air compressor, a heater and a flow meter, and the air compressor, the heater and the flow meter are sequentially arranged on the hot air input pipe along the hot air flow direction.
Further, a valve is arranged between the input unit and the solid-liquid separator.
Further, the output end of the solid-liquid separator is communicated with an output unit, and the output unit comprises a fluosilicic acid storage tank and a washing liquid storage tank.
Furthermore, be equipped with discharge gate and first waste gas export on the fluosilicic acid storage tank, be equipped with waste liquid export and second waste gas export on the washing liquid storage tank.
Further, a heat exchanger for recovering heat from the washing liquid and the off-gas is provided between the solid-liquid separator and the washing liquid storage tank.
Further, the solid-liquid separator comprises a filter cylinder, a stirring device and a filtering device, wherein the stirring device and the filtering device are positioned in the filter cylinder, and the filtering device is positioned at the lower part of the filter cylinder and is used for solid-liquid separation; the stirring device is positioned above the filtering device and is rotationally connected with the filtering cylinder for stirring the solid.
Furthermore, a lifting device for adjusting the height of the stirring device is arranged on the stirring device.
Further, a liquid level meter for detecting the height of the material in the filter cylinder is arranged on the filter cylinder.
The technical principle of the utility model is that:
the utility model discloses a mode that low pressure vapor blasts and washing liquid washing can get rid of the adsorbed fluorine element in silica powder surface. The utility model adopts the modes of water vapor heating and water vapor replacement to remove various forms of fluorine elements contained in the inner cavity of the silicon dioxide powder, on one hand, low-pressure water vapor heating expansion is adopted to vaporize and escape the fluorine content contained in the cavity; on the other hand, low-pressure steam enters the cavity inside the silicon dioxide powder and is liquefied, the fluorine element inside the silicon dioxide is replaced, and then the low-pressure steam is heated to enable liquid water to be vaporized and escaped, and meanwhile, the replaced fluorine element is taken away. Specifically, during the contact of water vapor or water with silica, a portion of the water molecules in the water vapor or water will be reacted with OH-And H+Attached to the silica surface, OH-With F in silica-Displacement occurs to achieve defluorination of the silica. At the same time, water vapor is continuously connected with silicon dioxide under low pressureIn the contact process, the water vapor also heats the silicon dioxide to lead the content of the silicon dioxide cavity to be vaporized and escape from the cavity, thereby realizing the reduction of the fluorine element in the content of the cavity. The silicon dioxide is washed, so that high-boiling-point impurities in the silicon dioxide can be further removed, and the heated silicon dioxide is cooled by the purified water, so that the gas in the silicon dioxide cavity is contracted due to cooling, and therefore negative pressure is generated, the purified water is sucked by the negative pressure, and further washing of the silicon dioxide cavity is realized. The drying aims to remove the water in the silicon dioxide and reduce the water content, thereby bringing convenience to the utilization of the silicon dioxide.
Compared with the prior art, the utility model discloses following beneficial effect has:
1) the mass fraction of fluorine element in the silicon dioxide product obtained by the system of the utility model is less than 0.5 percent, and the quality can reach the national standard of precipitated white carbon black;
2) the silicon dioxide product obtained by the system of the utility model has a large specific surface area and is at 180-phase 200m2About/g, good performance and high utilization value, and is beneficial to the next production and utilization;
3) the system has low production cost, reduces the discharge of solid wastes, protects the environment and is suitable for large-scale popularization.
4) The system can effectively separate the fluosilicic acid and the silicon dioxide mixed slurry, purify the silicon dioxide and effectively remove fluorine elements on the silicon dioxide.
Drawings
Fig. 1 is a front view of a separation and purification system in embodiment 1 of the present invention.
In the above drawings: 1. a barrel; 2. a cover body; 3. a filter plate; 4. a power assembly; 5. a stirrer; 6. a hydraulic lifting device 7 and a feed inlet; 8. a material input pipe; 9. a first valve; 10. a water vapor inlet; 11. a water vapor input pipe; 12. a second valve; 13. a first flow meter; 14. a washing liquid inlet; 15. a washing liquid input pipe; 16. a third valve; 17. drying the opening; 18. a hot air input pipe; 19. an air compressor; 20. a heater; 21. a fourth valve; 22. a second flow meter; 23. an output port; 24. a first output pipe; 25. a second output pipe; 26. a fifth valve; 27. a sixth valve; 28. a fluosilicic acid storage tank; 29. a washing liquid storage tank; 30. a first material outlet; 31. a first exhaust gas outlet; 32. a straight tube heat exchanger; 33. a liquid level meter; 34. a second material outlet; 35. a seventh valve; 36. a waste liquid outlet; 37. a second exhaust outlet.
Detailed Description
The technical solution of the present invention will be further explained with reference to the accompanying drawings and embodiments.
Example 1 separation and purification System for Fluorosilicic acid and silica Mixed slurry
A solid-liquid separator includes a filter cartridge, an agitation device and a filtering device disposed within the filter cartridge.
As shown in FIG. 1, the cartridge is cylindrical with a height of 2000mm and an internal diameter of 3600 mm. The filter cartridge comprises a cartridge body 1 and a cover body 2, wherein the cartridge body 1 is clamped with the cover body 2.
The filtering device is a cylindrical filtering plate 3 with the aperture size of 10 mu m and the diameter of 3600mm, the filtering plate 3 is horizontally arranged at the lower part of the filter cylinder, the periphery of the filtering plate 3 is tightly attached to the inner wall of the filter cylinder, so that liquid is filtered, and solid is trapped above the filtering plate 3.
The stirring device is a stirrer 5 and is positioned in the cylinder body 1; the lifting device is a hydraulic lifting device 6 and is positioned at the top of the cover body 2; the stirrer 5 and the hydraulic lifting device 6 are driven by a power assembly 4, and the power assembly 4 is connected to the top of the cover body 2 of the filter cartridge; the output shaft of the power assembly 4 is connected with a hydraulic lifting device 6 and a stirrer 5 in sequence. The hydraulic lifting device 6 is of a conventional design in the prior art and is used for lifting the stirrer 5; the stirrer 5 comprises a turbine stirrer, an axial flow stirrer and the like which are conventional in the prior art, and the stirrer 5 used in the embodiment is a turbine stirrer and is used for stirring and raking out materials.
The upper part of the filter cylinder is provided with a feed inlet 7, a steam inlet 10, a washing liquid inlet 14 and a drying port 17 which are positioned above the filter plate 3. The mixed slurry input unit is communicated with the feed inlet 7 through a material input pipe 8 and is used for inputting mixed slurry, and a first valve 9 is arranged on the material input pipe 8; the water vapor input unit is communicated with the water vapor inlet 10 through a water vapor input pipe 11 and is used for inputting low-pressure steam, and a second valve 12 and a first flowmeter 13 are sequentially arranged on the water vapor input pipe 11 along the water vapor input direction; the washing liquid input unit is communicated with a washing liquid inlet 14 through a washing liquid input pipe 15 and is used for inputting washing liquid, and a third valve 16 is arranged on the washing liquid input pipe 15; the hot air input unit is communicated with the drying port 17 through a hot air input pipe 18 and is used for inputting hot air, and an air compressor 19, a heater 20, a fourth valve 21 and a second flowmeter 22 are sequentially arranged on the hot air input pipe 18 along the hot air input direction; the air compressor 19 is used to compress air, and the heater 20 is used to heat the compressed air.
The bottom of the filter cylinder is provided with an output port 23 positioned below the filter plate 3, the output port 23 is respectively communicated with a first output pipe 24 and a second output pipe 25, the first output pipe 24 is provided with a fifth valve 26, and the first output pipe 24 is used for outputting materials and waste gas; the second output pipe 25 is provided with a sixth valve 27, and the second output pipe 25 is used for outputting waste liquid and waste gas. The free end of the first output pipe 24 is communicated with a fluosilicic acid storage tank 28, the bottom of the fluosilicic acid storage tank 28 is provided with a first material outlet 30, and the top is provided with a waste gas outlet 31; a fluorosilicic acid storage tank 28 is used to store filtered fluorosilicic acid. The second output pipe 25 is communicated with the washing liquid storage tank 29 through the straight pipe type heat exchanger 32, and the high-temperature washing liquid and the hot air output by the second output pipe 25 can exchange heat in the straight pipe type heat exchanger 32 to reduce the temperature, and then flow into the washing liquid storage tank 29. The bottom of the washing liquid storage tank 29 is provided with a waste liquid outlet 36, and the top is provided with a second waste gas outlet 31; the cover body 2 is provided with a liquid level meter 33 for displaying the height of the material in the cylinder body 1. And a second material outlet 34 is arranged at the position where the side wall of the cylinder body 1 is level with the filter plate 3 and is used for outputting the silicon dioxide solid.
The following steps are followed when in use:
s1: starting the hydraulic lifting device 6, and lifting the blades of the stirrer 5 to the highest set height of 600 mm; the first valve 9 is opened, and the mixed slurry of fluosilicic acid and silica is fed into the barrel 1 from the feed port 7. Fluosilicic acid flows out from the output port 23 through the filter plate 3, the fifth valve 26 is opened, and the fluosilicic acid enters the fluosilicic acid storage tank 28 through the first output pipe 24 for storage. The silicon dioxide is retained above the filter plate 3, when the retention amount of the silicon dioxide reaches 500mm (about 800kg), the injection of the mixed slurry of the fluosilicic acid and the silicon dioxide is stopped, and the first valve 9 is closed;
s2: lowering the stirrer 5 to the height of 500mm of the silicon dioxide stacking height, starting the power assembly 4, adjusting the stirring speed to 5r/min, leveling the height of the silicon dioxide solid stacking body, simultaneously opening the second valve 12, sending 150 ℃ water vapor into the filter cylinder from the water vapor inlet 10, carrying out water vapor purification on the silicon dioxide, setting the sending amount of the water vapor to be 4000kg, the purification time to be 30min, stopping sending the water vapor after the set value is reached, closing the second valve 12, and carrying out water vapor purification on the silicon dioxide solid in the filter cylinder. Opening a fifth valve 26, discharging the fluorine-containing waste gas from an output port 23, entering a fluosilicic acid storage tank 28 through a first output pipe 24, discharging the fluorine-containing waste gas from a first waste gas outlet 31 at the top of the fluosilicic acid storage tank 28, and closing the fifth valve 26;
s3: keeping the stirrer 5 in a moving state, opening the third valve 16, feeding purified water into the filter cylinder from the washing liquid inlet 14, stopping feeding the purified water when the liquid level in the filter cylinder reaches 1000mm, and closing the third valve 16; the stirrer 5 is lowered to a height of 20mm, the stirring speed is kept at 5r/min, the stirring temperature is 60 ℃, and the stirring time reaches 30 min. Opening the sixth valve 27, discharging the washing liquid from the output port 23, flowing into the straight-tube heat exchanger 32 through the second output tube 25 for heat exchange, then flowing into the washing liquid storage tank 29 for storage, and closing the sixth valve 27;
s4: and (3) lifting the stirrer 5 to 500mm, opening the second valve 12, feeding steam with the temperature of 150 ℃ into the filter cylinder from the steam inlet 10, performing secondary steam purification on the silicon dioxide, setting the feeding amount of the steam to be 4000kg, and the purification time to be 30min, stopping feeding the steam after the set value is reached, closing the second valve 12, and performing steam purification on the silicon dioxide solid in the filter cylinder. Opening a fifth valve 26, discharging the fluorine-containing waste gas from an output port 23, entering a fluosilicic acid storage tank 28 through a first output pipe 24, discharging the fluorine-containing waste gas from a first waste gas outlet 31 at the top of the fluosilicic acid storage tank 28, and closing the fifth valve 26;
s5: opening a fourth valve 21, starting an air compressor 19 and a heater 20, compressing and heating air, sending hot air heated to 80 ℃ into the filter cylinder from the drying port 17 until the temperature of an output port 23 reaches 80 ℃, and drying the silicon dioxide purified by the secondary water vapor; the waste gas is discharged from the output port 23, flows into the straight pipe type heat exchanger 32 through the second output pipe 25 for heat exchange, enters the washing liquid storage tank 29, and is discharged from a second waste gas outlet 37 at the top of the washing liquid storage tank 29;
the stirring speed is kept at 5r/min, the seventh valve 35 is opened, the blades of the stirrer 5 are slowly reduced to a minimum of 10mm, and the silica product is raked out of the solid-liquid separator through the second material outlet 34.
In this example, 800kg by weight of amorphous silica product having a fluorine content of 0.3% per batch was obtained. The specific surface area of the material is 180m determined by a nitrogen adsorption method2/g。
Finally, although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that the present invention can be modified or replaced by other means without departing from the spirit and scope of the present invention, which should be construed as limited only by the appended claims.
Claims (10)
1. A separation and purification system for fluosilicic acid and silicon dioxide mixed slurry is characterized by comprising a solid-liquid separator and an input unit, wherein the solid-liquid separator is used for separating fluosilicic acid and silicon dioxide, the input end of the solid-liquid separator is communicated with the input unit,
the input unit comprises a water vapor input unit, a washing liquid input unit and a mixed slurry input unit;
the steam input unit is used for conveying steam into the solid-liquid separator to purify the silicon dioxide;
the washing liquid input unit is used for conveying washing liquid into the solid-liquid separator to wash the silicon dioxide;
and the mixed slurry input unit is used for conveying the fluosilicic acid and the silicon dioxide into the solid-liquid separator.
2. The system of claim 1, wherein the input unit further comprises a hot air input unit, which is communicated with the solid-liquid separator through a hot air input pipe, for delivering hot air into the solid-liquid separator to dry the silica.
3. The separation and purification system for a fluosilicic acid and silica mixed slurry according to claim 2, wherein the hot air input unit comprises an air compressor, a heater and a flow meter, which are arranged on the hot air input pipe in sequence along a hot air flow direction.
4. The system for separating and purifying a mixed slurry of fluosilicic acid and silica according to claim 1, wherein a valve is provided between the input unit and the solid-liquid separator.
5. A separation and purification system for a fluosilicic acid and silica mixed slurry according to claim 1, wherein an output end of the solid-liquid separator is communicated with an output unit, and the output unit comprises a fluosilicic acid storage tank and a washing liquid storage tank.
6. The separation and purification system for a fluosilicic acid and silica mixed slurry according to claim 5, wherein a discharge port and a first waste gas outlet are provided on the fluosilicic acid storage tank, and a waste liquid outlet and a second waste gas outlet are provided on the washing liquid storage tank.
7. A separation and purification system for a fluosilicic acid and silica mixed slurry according to claim 6, wherein a heat exchanger for recovering heat from the washing liquid and the off-gas is provided between said solid-liquid separator and the washing liquid storage tank.
8. The system for separating and purifying a mixed slurry of fluosilicic acid and silica according to claim 1, wherein the solid-liquid separator comprises a filter cylinder, an agitating device and a filtering device, wherein the agitating device and the filtering device are positioned in the filter cylinder, and the filtering device is positioned at the lower part of the filter cylinder and is used for solid-liquid separation; the stirring device is positioned above the filtering device and is rotationally connected with the filter cylinder for stirring the solid.
9. The system for separating and purifying a mixed slurry of fluosilicic acid and silica according to claim 8, wherein the stirring device is provided with a lifting device for adjusting the height of the stirring device.
10. The system of claim 8, wherein a level gauge is disposed on the filter cartridge for measuring the level of material in the filter cartridge.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202220400424.7U CN216825200U (en) | 2022-02-25 | 2022-02-25 | Separation and purification system for fluosilicic acid and silicon dioxide mixed slurry |
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| Application Number | Priority Date | Filing Date | Title |
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| CN202220400424.7U CN216825200U (en) | 2022-02-25 | 2022-02-25 | Separation and purification system for fluosilicic acid and silicon dioxide mixed slurry |
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| CN216825200U true CN216825200U (en) | 2022-06-28 |
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| CN202220400424.7U Active CN216825200U (en) | 2022-02-25 | 2022-02-25 | Separation and purification system for fluosilicic acid and silicon dioxide mixed slurry |
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| CB03 | Change of inventor or designer information |
Inventor after: He Haoming Inventor after: Gong Xingrong Inventor after: Wang Fei Inventor before: He Minghao Inventor before: Gong Xingrong Inventor before: Wang Fei |
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| CB03 | Change of inventor or designer information |