CN109107221B - A solid-liquid extraction purification device and purification method - Google Patents
A solid-liquid extraction purification device and purification method Download PDFInfo
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- CN109107221B CN109107221B CN201810952883.4A CN201810952883A CN109107221B CN 109107221 B CN109107221 B CN 109107221B CN 201810952883 A CN201810952883 A CN 201810952883A CN 109107221 B CN109107221 B CN 109107221B
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- 238000000746 purification Methods 0.000 title claims abstract description 62
- 238000000956 solid--liquid extraction Methods 0.000 title claims description 39
- 238000000034 method Methods 0.000 title claims description 21
- 239000007788 liquid Substances 0.000 claims abstract description 120
- 238000000605 extraction Methods 0.000 claims abstract description 109
- 238000005406 washing Methods 0.000 claims abstract description 69
- 239000011347 resin Substances 0.000 claims abstract description 52
- 229920005989 resin Polymers 0.000 claims abstract description 52
- 239000007787 solid Substances 0.000 claims abstract description 36
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000000203 mixture Substances 0.000 claims abstract description 17
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 12
- 230000000149 penetrating effect Effects 0.000 claims abstract description 7
- 238000003860 storage Methods 0.000 claims description 66
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 25
- 239000007789 gas Substances 0.000 claims description 19
- 239000008367 deionised water Substances 0.000 claims description 17
- 229910021641 deionized water Inorganic materials 0.000 claims description 17
- 238000010926 purge Methods 0.000 claims description 7
- 239000002184 metal Substances 0.000 claims description 5
- 238000005086 pumping Methods 0.000 claims description 4
- 238000009423 ventilation Methods 0.000 claims description 3
- 238000007664 blowing Methods 0.000 claims description 2
- 229910001873 dinitrogen Inorganic materials 0.000 claims description 2
- 238000010438 heat treatment Methods 0.000 claims description 2
- 238000002360 preparation method Methods 0.000 claims description 2
- 239000011148 porous material Substances 0.000 claims 4
- 230000007423 decrease Effects 0.000 claims 2
- 230000000694 effects Effects 0.000 abstract description 14
- 239000000463 material Substances 0.000 abstract description 11
- 150000003839 salts Chemical class 0.000 abstract description 3
- 239000002904 solvent Substances 0.000 abstract description 3
- 239000000843 powder Substances 0.000 description 11
- 239000012535 impurity Substances 0.000 description 5
- 238000007599 discharging Methods 0.000 description 4
- 150000003457 sulfones Chemical class 0.000 description 4
- 238000009826 distribution Methods 0.000 description 3
- 238000002474 experimental method Methods 0.000 description 3
- 239000002245 particle Substances 0.000 description 3
- 210000003437 trachea Anatomy 0.000 description 3
- 238000005119 centrifugation Methods 0.000 description 2
- 150000001875 compounds Chemical class 0.000 description 2
- 230000003247 decreasing effect Effects 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 238000004321 preservation Methods 0.000 description 2
- 238000004062 sedimentation Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 238000004140 cleaning Methods 0.000 description 1
- 238000007667 floating Methods 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000002386 leaching Methods 0.000 description 1
- 238000000622 liquid--liquid extraction Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 239000013557 residual solvent Substances 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 229910001220 stainless steel Inorganic materials 0.000 description 1
- 239000010935 stainless steel Substances 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D11/00—Solvent extraction
- B01D11/02—Solvent extraction of solids
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- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Extraction Or Liquid Replacement (AREA)
Abstract
A plurality of first annular air pipes are arranged in an extraction tower at intervals from top to bottom, a plurality of first air holes with upward openings are arranged on each first annular air pipe at intervals, all the first annular air pipes are communicated with a first air inlet pipe penetrating the extraction tower, nitrogen is introduced into the first air inlet pipe, then flows into each first annular air pipe, and is sprayed upwards through the first air holes on the first annular air pipes, so that the sprayed nitrogen and downward flowing liquid are impacted together, turbulence of a solid-liquid mixture is enhanced, the mass transfer rate is improved, the contact area of solid resin and washing liquid is increased, and solvents and salts in the resin are fully dissolved in the washing liquid, so that the washing effect is improved, and the purification rate is increased; the second annular air pipes are arranged below each first annular air pipe in a matched mode, and can sweep washed materials, so that the liquid content in the materials is greatly reduced.
Description
Technical Field
The invention relates to the field of polymer material preparation, in particular to a solid-liquid extraction purification device and a purification method.
Background
Extraction is often used in chemical experiments and its operation does not cause a change in the chemical composition of the extracted material, so that the extraction operation is a physical process, extraction being one of the means used in organic chemistry laboratories to purify and purify compounds by which the desired compounds can be extracted from solids or liquids. Extraction is often divided into solid-liquid extraction and liquid-liquid extraction, wherein for solid-liquid extraction, which is also called leaching, a solvent is used to separate impurity components in a solid mixture, currently, for solid-liquid extraction, an intermittent kettle type purification method is generally adopted in the industry to repeatedly wash for many times, after each washing is completed, powder is required to be returned to a kettle to be added with water for washing again, repeated washing and centrifugation are required, and the purification is completed in the same kettle, so that the purification efficiency is very low (the washing time is as long as 30-40 hours), water consumption is high, for example, after the sulfone resin is polymerized, the reacted solution is injected into water to be solidified, and then the solidified solid-liquid mixture is crushed into a solid-liquid mixture with solid matters in powder form through a crushing process.
In order to solve the problems, the technical personnel in the industry propose that the purification efficiency of solid-liquid extraction can be improved and the water consumption can be reduced, namely, a tower type extraction device is adopted, and the purification of solid resin is carried out in a countercurrent extraction mode through a natural sedimentation experiment, but the sulfone resin needs to be crushed into powder before being purified, so that the sulfone resin powder has small particle size and uneven distribution, the distribution is different from 20 um to 3mm, the stacking density is 0.2g/ml to 0.4 g/ml, a large amount of powder with small particle size floats on the liquid surface in the natural sedimentation experiment, and the contact area between the powder floating on the liquid surface and the washing liquid is small when the countercurrent extraction mode is adopted, so that the washing effect is poor and the purification rate is low.
Disclosure of Invention
The invention aims to provide a solid-liquid extraction purification device and a purification method, which can effectively improve the extraction efficiency of solid-liquid extraction and reduce the water consumption, and can greatly improve the purification rate of powdery resin formed by a crushing process.
The invention relates to a solid-liquid extraction purification device, which comprises an extraction tower and a plurality of storage tanks, wherein each storage tank is respectively communicated with the bottom of the extraction tower through a pipeline and is respectively communicated with the same vacuum pump through a pipeline, the bottom of each storage tank is respectively communicated with the same centrifugal pump through a pipeline, and the centrifugal pump is also communicated with the top of the extraction tower through a pipeline; a plurality of first annular air pipes are arranged in the extraction tower at intervals from top to bottom, a plurality of first air holes with upward openings are arranged on each first annular air pipe at intervals, and all the first annular air pipes are communicated with a first air inlet pipe penetrating through the extraction tower; a second annular air pipe is arranged below each first annular air pipe and inside the extraction tower, a plurality of second air holes with downward openings are arranged on each second annular air pipe at intervals, and all the second annular air pipes are communicated with a second air inlet pipe penetrating through the extraction tower; a feed liquid inlet is arranged on the side wall of the upper part of the extraction tower; the bottom of the extraction tower is provided with a filter plate which can be opened and closed relative to the extraction tower.
The invention relates to a solid-liquid extraction and purification method, which comprises the following steps:
1) Before solid-liquid extraction and purification, numbering a plurality of storage tanks, setting a first storage tank as an empty tank, putting deionized water into a storage tank with the last number, putting a plurality of storage tanks in the middle into washing liquid, and sequentially decreasing the concentration of the washing liquid in each storage tank from a second storage tank;
2) Starting a vacuum pump, injecting a resin solid-liquid mixture to be purified in a liquid tank into an extraction tower through a liquid inlet on the extraction tower by a liquid pump, wherein liquid enters a first storage tank after being filtered by a filter plate at the bottom of the extraction tower, and solid resin is left in the extraction tower, and after the resin solid-liquid mixture is conveyed, introducing nitrogen into a second annular air pipe through a second air inlet pipe to purge the solid resin;
3) Discharging the liquid in the first storage tank, and stopping ventilation to the second air inlet pipe;
4) Starting a vacuum pump and a centrifugal pump, pumping the washing liquid in a second storage tank with highest washing liquid concentration through the centrifugal pump, injecting the washing liquid into the extraction tower from the top of the extraction tower, introducing nitrogen into a first annular air pipe through a first air inlet pipe, then flowing the liquid in the extraction tower 1 into a first storage tank, and discharging the gas through the vacuum pump;
5) Stopping air supply of the first air inlet pipe, starting the second air inlet pipe, introducing nitrogen into each second annular air pipe, and purging the solid resin to finish one-time washing;
6) And (3) repeating the step (4) and the step (5), after each washing, the liquid in the extraction tower flows into the storage tank emptied in the previous step, and after all the washing liquid in the storage tank containing the washing liquid and the deionized water in the storage tank with the last number are used, the filter plate at the bottom of the extraction tower is opened, the solid resin is extracted to the next process link, and the purification of the solid resin is completed.
According to the solid-liquid extraction purification device and the purification method, the plurality of storage tanks are arranged, meanwhile, one storage tank is set to be an empty tank, deionized water is put into the other storage tank, washing liquids with different concentrations are put into the other storage tank, the purification of solid resin can be completed through the purification method, and the washing liquid used each time and the deionized water used last are stored into the previous storage tank and can be used for purifying a resin solid-liquid mixture to be purified next time; each time the liquid in the reservoir tank, which is preset as an empty tank, is discharged, it is ready for the next pumping of liquid. The washing liquid in the storage tanks can be reused, and deionized water is only needed to be injected into one storage tank in each round of washing, so that the water consumption is greatly reduced, the production cost is reduced, and meanwhile, the operation of repeated washing and then centrifugation is not needed, so that the purification working efficiency is greatly improved. Because a plurality of first annular air pipes are arranged in the extraction tower from top to bottom at intervals, a plurality of first air holes with upward openings are arranged on each first annular air pipe at intervals, all the first annular air pipes are communicated with a first air inlet pipe penetrating the extraction tower, nitrogen is introduced into the first air inlet pipe, then flows into each first annular air pipe, and is sprayed upwards through the first air holes on the first annular air pipes, so that the sprayed nitrogen and downward flowing liquid are impacted together, the turbulence of a solid-liquid mixture is enhanced, the mass transfer rate is improved, the contact area of solid resin and washing liquid is increased, and the solvent and salt in the resin are fully dissolved in the washing liquid, so that the washing effect is improved, and the purification rate is increased; and all be provided with the second annular trachea in extraction tower inside in every first annular tracheal below, all the interval is provided with a plurality of opening second gas pockets downwards on every second annular trachea, all second annular trachea all with run through extraction tower's second intake pipe intercommunication, can be when letting in nitrogen gas to the second intake pipe to purge the material, thereby reduce the liquid content in the material by a wide margin. Therefore, the solid-liquid extraction and purification device can greatly improve the purification rate and the purification efficiency of the solid resin, and meanwhile, the washing liquid can be recycled, so that the water consumption can be reduced, and the device is energy-saving and environment-friendly. In addition, because the first annular air pipe is arranged, the turbulence of the solid-liquid mixture can be enhanced, the mass transfer rate is improved, the contact area of solid resin and washing liquid is increased, and meanwhile, because the second annular air pipe is arranged, the washed material can be purged, and the water content of the material is further reduced, the method is very suitable for purifying the powder resin solid-liquid mixture material after the crushing process, and the purification rate and the purification efficiency are higher, for example, the purification of sulfone resin.
Drawings
FIG. 1 is a schematic diagram of the structure of the present invention.
FIG. 2 is a schematic diagram of the structure of the extraction column according to the present invention.
Fig. 3 is a partial enlarged view of a portion a in fig. 2.
Fig. 4 is a top view of the first and second annular air tubes of the present invention.
Fig. 5 is a front view of fig. 4.
Detailed Description
The solid-liquid extraction purification device comprises an extraction tower 1 and a plurality of storage tanks 2, wherein each storage tank 2 is respectively communicated with the bottom of the extraction tower 1 through a pipeline and is respectively communicated with the same vacuum pump 13 through a pipeline, the bottom of each storage tank 2 is respectively communicated with the same centrifugal pump 3 through a pipeline, and the centrifugal pump 3 is also communicated with the top of the extraction tower 1 through a pipeline; a plurality of first annular air pipes 4 are arranged in the extraction tower 1 at intervals from top to bottom, a plurality of first air holes 5 with upward openings are arranged on each first annular air pipe 4 at intervals, and all the first annular air pipes 4 are communicated with a first air inlet pipe 6 penetrating through the extraction tower 1; a second annular air pipe 7 is arranged below each first annular air pipe 4 and inside the extraction tower 1, a plurality of second air holes 8 with downward openings are arranged on each second annular air pipe 7 at intervals, and all the second annular air pipes 7 are communicated with a second air inlet pipe 9 penetrating through the extraction tower 1; a feed liquid inlet 18 is arranged on the upper side wall of the extraction tower 1; a filter plate 10 which can be opened and closed relative to the extraction column 1 is arranged at the bottom of the extraction column 1. The shapes of the first air holes 5 and the second air holes 8 can be arbitrarily selected from round, conical or square, and the like, and the first annular air pipe 4 and the second annular air pipe 7 are made of stainless steel.
The directions of the openings of the two adjacent first air holes 5 on the first annular air pipe 4 are staggered according to angles, such as the directions of the openings are staggered by 5 degrees, 10 degrees, 15 degrees, 20 degrees, 25 degrees, 30 degrees or 45 degrees, and the like, and the directions of the openings of the two adjacent second air holes 8 on the second annular air pipe 7 are staggered according to actual needs, such as the directions of the openings are staggered by 5 degrees, 10 degrees, 15 degrees, 20 degrees, 25 degrees, 30 degrees or 45 degrees, and the like, and the directions of the openings are selected according to actual needs. By arranging the opening directions of the adjacent holes to be staggered according to angles, the sprayed gas can be sprayed towards all directions, and when the first annular air pipe 4 is sprayed, the sprayed gas can be impacted with liquid in all directions, so that turbulence can be generated at all positions of the liquid, the mass transfer rate is further increased, and the contact area between the solid resin and the washing liquid is increased; when the second annular air pipe 7 is used for air injection, the second annular air pipe can be contacted with the solid resin in all directions, and the solid resin can be purged from all directions, so that the liquid content in the material is further greatly reduced.
The aperture of the first air hole 5 and the aperture of the second air hole 8 are both 0.5 mm-8 mm, such as 0.5mm、0.6mm、0.9mm、1m、1.3mm、1.5mm、2mm、2.4mm、2.8mm、3mm、3.5mm、3.8mm、4mm、4.6mm、5mm、5.5mm、6mm、6.5mm、7mm、7.8mm mm or 8mm, and preferably 2 mm-5 mm, and by determining the aperture of the first air hole 5 and the aperture of the second air hole 8, stronger turbulence can be generated when the gas blown out from the first air hole 5 contacts with the liquid within the aperture range, so that the mass transfer effect between the washing liquid and the solid resin is more sufficient, and the cleaning effect is better; the residual liquid containing impurities in the solid resin can be blown out more effectively due to the gas blown out by the second air holes 8.
Nozzles are arranged on the first air holes 5 and the second air holes 8 so as to increase the strength of gas spraying.
The space between every two adjacent first annular air pipes 4 is 300 mm-1000 mm, such as 300mm, 350mm, 400mm, 450mm, 500mm, 550mm, 600mm, 650mm, 700mm, 750mm, 800mm, 850mm, 900mm, 950mm or 1000mm, and the like, preferably 500 mm-700 mm; the distance between adjacent second annular air pipes 7 is 300 mm-1000 mm, such as 300mm, 350mm, 400mm, 450mm, 500mm, 550mm, 600mm, 650mm, 700mm, 750mm, 800mm, 850mm, 900mm, 950mm or 1000mm, etc., preferably 500 mm-700 mm. In the process that the solid resin flows downwards along with the liquid, the liquid forms larger air resistance to the air flow blown out by the first air hole, the air pressure drop is larger, and after the solid resin moves in the tower for a certain distance, the mass transfer effect on the solid resin and the washing liquid is obviously reduced, so that the washing effect and the residual liquid removal effect can be ensured by arranging the first annular air pipe 4 and the second annular air pipe 7 at a certain distance, and the distance between the adjacent first annular air pipe 4 and the adjacent second annular air pipe 7 is determined within the range, so that the washing effect and the residual liquid removal effect can be further ensured.
The distance between the last two adjacent first annular air pipes 4 near the bottom of the extraction tower 1 is 300mm, and the distance between the last two adjacent second annular air pipes 7 near the bottom of the extraction tower 1 is 300mm. Because the gravity action of solid resin and washing liquid, the bulk density of the material at the bottom of the extraction tower 1 is higher than that of the material at the upper part, and the pressure drop of the gas at the section is larger, therefore, the space between the adjacent first annular air pipes 4 and the adjacent second annular air pipes 7 is reduced at the section, and the washing effect and the residual liquid removing effect can be better ensured.
The diameters of the inner parts of the pipelines of the first annular air pipe 4 and the second annular air pipe 7 are 15 mm-25 mm, such as 15mm, 16mm, 17mm, 18mm, 19mm, 20mm, 21mm, 22mm, 23mm, 24mm or 25mm, and the diameters of the circular rings are 300 mm-600 mm, such as 300mm, 350mm, 400mm, 450mm, 500mm, 550mm or 600 mm.
The metal filter screens 11 are arranged on the first annular air pipe 4, the second annular air pipe 7 and the filter plate 10, and the mesh number of the metal filter screens 11 is 200-500 meshes, such as 200-250 meshes, 300 meshes, 350 meshes, 400 meshes, 450 meshes or 500 meshes. Since the particle size range distribution of the resin powder is wide, the metal screen 11 is provided to prevent the first air holes 5 or the second air holes 8 from being blocked by the minute resin powder.
The filter 10 is hinged at a bottom surface through hole of the extraction tower 1, a hydraulic driving mechanism for controlling the opening and closing of the filter relative to the extraction tower 1 is connected to the filter, the hydraulic driving mechanism comprises a hydraulic cylinder 14 vertically arranged on the outer side wall of the extraction tower 1, a telescopic shaft of the hydraulic cylinder 14 is vertically downward, a first connecting rod 15 is hinged to the free end of the telescopic shaft of the hydraulic cylinder 14, the free end of the first connecting rod 15 is fixedly connected to a rotating shaft 16 capable of rotating relative to the extraction tower 1, a second connecting rod 17 capable of rotating along with the rotating shaft is further connected to the rotating shaft 16, and the free end of the second connecting rod 17 is fixedly connected with the lower surface of the filter 10. The telescopic shaft of the hydraulic cylinder 14 stretches out, so that the telescopic shaft drives the first connecting rod 15 to swing downwards, the first connecting rod 15 drives the rotating shaft 16 to rotate, so that the rotating shaft 16 drives the second connecting rod 17 to swing upwards, the filter plate 10 is tightly covered at the bottom of the extraction tower 1, the telescopic shaft of the hydraulic cylinder 14 retracts, so that the telescopic shaft drives the first connecting rod 15 to swing upwards, the first connecting rod 15 drives the rotating shaft 16 to rotate, and the rotating shaft 16 drives the second connecting rod 17 to swing downwards, so that the filter plate 10 is opened relative to the bottom of the extraction tower 1. The opening and closing of the filter plate 10 are convenient to control, the structure is simple, and the operation is convenient.
The diameter of the extraction tower 1 is 500 mm-1200 mm, such as 500mm, 550mm, 600mm, 650mm, 700mm, 750mm, 800mm, 850mm, 900mm, 950mm, 1000mm, 1050mm, 1100mm, 1150mm or 1200mm, and the like, preferably 600 mm-800 mm; the height of the extraction tower 1 is 10 m-15 m, such as 10m, 11m, 12m, 13m, 14m or 15m, etc.
A liquid distributor 12 for injecting washing liquid and deionized water is arranged on the top opening of the extraction tower 1, the washing liquid or the deionized water pumped by the centrifugal pump 3 flows into the extraction tower 1 from the liquid distributor 12 at the top of the extraction tower 1, so that the flowing washing liquid or the flowing deionized water can be uniformly distributed in the extraction tower 1, and the solid resin in the extraction tower 1 is effectively ensured to be fully contacted with the washing liquid and the deionized water for effective purification; in addition, the liquid distributor 12 is arranged at the top of the extraction tower 1, so that the height of the liquid distributor 12 is higher than that of the feed liquid inlet 18, and the solid-liquid mixture can flow into the extraction tower 1 completely, so that the solid resin is prevented from being intercepted and not entering the extraction tower 1 when the solid-liquid mixture flows through the liquid distributor 12. The liquid distributor 12 is commercially available.
The outer wall of the extraction tower 1 is wrapped with the heat preservation layer, and the solubility of impurities contained in the solid resin in the washing liquid increases along with the temperature rise, so that the temperature of the washing liquid in the extraction tower 1 is more stable by wrapping the heat preservation layer on the outer wall of the extraction tower 1 in order to ensure the washing effect.
A heating coil is arranged in each storage tank 2, so that the washing liquid can be heated, the solubility of impurities in the solid resin in the washing liquid is improved, and the washing effect is enhanced. And the temperature value is actually controlled according to the temperature required by the solubility of different impurities.
A solid-liquid extraction purification method comprises the following steps: (1) Before solid-liquid extraction and purification, numbering a plurality of storage tanks 2, setting a first storage tank 2 as an empty tank, putting deionized water into the storage tank 2 with the last number, putting a plurality of storage tanks 2 in the middle into washing liquid, and sequentially decreasing the concentration of the washing liquid in each storage tank 2 from a second storage tank 2; the number modes of the plurality of storage tanks 2 are various, and the embodiment is only one of the number modes, and when the number is different, only the liquid is controlled to enter the corresponding storage tank 2 through a program; (2) Starting a vacuum pump 13, injecting a solid-liquid mixture to be purified in a liquid tank 19 into the extraction tower 1 through a liquid inlet 18 on the extraction tower 1 by a liquid pump 20, wherein liquid enters a first storage tank 2 after being filtered by a filter plate 10 at the bottom of the extraction tower 1, and solid resin is left in the extraction tower 1, and after the solid-liquid mixture is conveyed, introducing nitrogen into a second annular air pipe 7 through a second air inlet pipe 9 to purge the solid resin; (3) Discharging the liquid in the first tank 2 and stopping ventilation to the second intake pipe 9; (4) Starting a vacuum pump 13 and a centrifugal pump 3, pumping the washing liquid in a second storage tank 2 with the highest concentration of the washing liquid through the centrifugal pump 3, injecting the washing liquid into the extraction tower 1 from the top of the extraction tower 1, introducing nitrogen into a first annular air pipe 4 through a first air inlet pipe 6, then flowing the liquid in the extraction tower 1 into a first storage tank 2, and discharging the gas through the vacuum pump; (5) Stopping supplying air to the first air inlet pipe 6, starting the second air inlet pipe 9, introducing nitrogen into each second annular air pipe 7, and purging the solid resin to finish one-time washing; (6) And (3) repeating the step (4) and the step (5), after each washing, flowing the liquid in the extraction tower 1 into the storage tank 2 emptied before until all the washing liquid in the storage tank 2 containing the washing liquid and the deionized water in the storage tank 2 with the last number are used, opening the filter plate 10 at the bottom of the extraction tower 1, extracting the solid resin to the next process link, and finishing the purification of the solid resin.
The flow rate of the washing liquid flowing into the extraction column 1 in the step (2) and the step (5) is 3m 3/h~6 m3/h, such as 3m 3/h、3.5 m3/h、4 m3/h、4.5 m3/h、5 m3/h、5.5 m3/h or 6m 3/h, etc.
In step (2) and step (5), the gas flow rate in the first annular gas pipe 4 is 1.5m 3/h ~3.5m3/h, such as 1.5m 3/h、2 m3/h、2.5 m3/h、3 m3/h or 3.5 m 3/h, etc.
In the step (3), the gas flow in the second annular gas pipe 7 is 20m 3/h~30 m3/h, such as 20m 3/h、22 m3/h、24 m3/h、25 m3/h、28 m3/h or 30 m 3/h, and the blowing duration is 10 min-20 min, such as 10min, 12min, 15min, 17min, 18min, 19min or 20min, etc. The liquid content in the resin powder can be reduced to below 50%.
Through the control of the gas flow and the washing liquid flow and the final washing of the deionized water, the residual solvent and salt in the resin powder can be thoroughly washed, the product quality is ensured to meet the requirements, and the purification rate is high.
Claims (20)
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| CN201810952883.4A CN109107221B (en) | 2018-08-21 | 2018-08-21 | A solid-liquid extraction purification device and purification method |
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| CN201810952883.4A CN109107221B (en) | 2018-08-21 | 2018-08-21 | A solid-liquid extraction purification device and purification method |
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| CN109107221B true CN109107221B (en) | 2024-11-19 |
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| CN205853163U (en) * | 2016-06-17 | 2017-01-04 | 江阴市博生新材料科技有限公司 | A kind of polyarylate resin pelletizing production line |
| CN206473861U (en) * | 2017-02-18 | 2017-09-08 | 江西天宇化工有限公司 | A kind of four chloropropanes/pentachloropropane water washing device |
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| CN202277731U (en) * | 2011-10-11 | 2012-06-20 | 大连百傲化学有限公司 | Multifunctional filtering and washing facility |
| CN203971523U (en) * | 2014-08-15 | 2014-12-03 | 苏州永添设备有限公司 | Automatic discharge improved structure of filter vat |
| CN206762351U (en) * | 2017-05-03 | 2017-12-19 | 安徽得奇环保科技股份有限公司 | The efficient back washing device of sandfiltration pot |
| CN114602876A (en) * | 2022-03-09 | 2022-06-10 | 山东明化新材料有限公司 | High molecular resin washing, separating and purifying method |
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