CN110585757A - Circulation continuous crystallizer - Google Patents
Circulation continuous crystallizer Download PDFInfo
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- CN110585757A CN110585757A CN201910955126.7A CN201910955126A CN110585757A CN 110585757 A CN110585757 A CN 110585757A CN 201910955126 A CN201910955126 A CN 201910955126A CN 110585757 A CN110585757 A CN 110585757A
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- 239000013078 crystal Substances 0.000 claims abstract description 115
- 239000007788 liquid Substances 0.000 claims abstract description 109
- 238000002425 crystallisation Methods 0.000 claims abstract description 71
- 230000008025 crystallization Effects 0.000 claims abstract description 71
- 238000010438 heat treatment Methods 0.000 claims abstract description 62
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 238000001914 filtration Methods 0.000 claims abstract description 21
- 238000007599 discharging Methods 0.000 claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 13
- 239000007787 solid Substances 0.000 claims abstract description 9
- 239000012530 fluid Substances 0.000 claims abstract description 6
- 238000009413 insulation Methods 0.000 claims abstract description 6
- 239000011229 interlayer Substances 0.000 claims description 23
- 239000002994 raw material Substances 0.000 claims description 11
- 238000000926 separation method Methods 0.000 claims description 11
- 239000000463 material Substances 0.000 claims description 8
- 239000000203 mixture Substances 0.000 claims description 7
- 230000003134 recirculating effect Effects 0.000 claims 1
- 239000012452 mother liquor Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 2
- 238000000034 method Methods 0.000 description 14
- DIZPMCHEQGEION-UHFFFAOYSA-H aluminium sulfate (anhydrous) Chemical compound [Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O DIZPMCHEQGEION-UHFFFAOYSA-H 0.000 description 10
- 239000012295 chemical reaction liquid Substances 0.000 description 4
- AMVQGJHFDJVOOB-UHFFFAOYSA-H aluminium sulfate octadecahydrate Chemical compound O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.O.[Al+3].[Al+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O AMVQGJHFDJVOOB-UHFFFAOYSA-H 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000005265 energy consumption Methods 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000012809 cooling fluid Substances 0.000 description 1
- 229910052593 corundum Inorganic materials 0.000 description 1
- 230000008021 deposition Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000005485 electric heating Methods 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 239000010410 layer Substances 0.000 description 1
- 239000004973 liquid crystal related substance Substances 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000004062 sedimentation Methods 0.000 description 1
- 239000008247 solid mixture Substances 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 229910001845 yogo sapphire Inorganic materials 0.000 description 1
Classifications
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0018—Evaporation of components of the mixture to be separated
- B01D9/0031—Evaporation of components of the mixture to be separated by heating
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D2009/0086—Processes or apparatus therefor
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- Chemical & Material Sciences (AREA)
- Crystallography & Structural Chemistry (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The application discloses a circulating continuous crystallizer, which comprises a top heating chamber, a middle crystallizing chamber, a bottom crystal collecting chamber, a filtering separator and a mother liquor return pipe, wherein the outer side of the top heating chamber is provided with a heat insulation sleeve; the top heating chamber is provided with a Venturi feeding pipe, a stirring device and a heating device, and the outer side of the middle crystallization chamber is provided with a gradient cooling device; a flow guide pipe is arranged in the middle crystallization chamber, a plurality of through holes are uniformly formed in the ring wall of the flow guide pipe, and a channel for fluid circulation is formed between the outer side wall of the flow guide pipe and the inner side wall of the middle crystallization chamber; a crystal liquid discharging pipe is arranged at the bottom of the bottom crystal collecting chamber and is connected with the filtering separator through the crystal liquid discharging pipe, and a solid outlet of the filtering separator discharges a crystal product; the liquid outlet of the filtering separator is divided into two paths, one path discharges mother liquid, and the other path is communicated with the lower end opening of the flow guide pipe through a mother liquid return pipe. The device has better crystallization treatment effect particularly for a solid-liquid crystallization system which is sensitive to temperature and small in metastable zone.
Description
Technical Field
The application relates to a circulating continuous crystallizer.
Background
The purification of the product is usually carried out during the production of aluminum sulfate octadecahydrate by crystallization. Because the product contains crystal water, the crystallization process is sensitive to temperature, the crystallization metastable zone is small, the traditional intermittent crystallization process has long operation time, easy outbreak of nucleation, small crystallization force and low product quality. If a continuous crystallization mode can be adopted in the crystallization process and the temperature of each part of the crystallization equipment is controllable, the aluminum sulfate octadecahydrate can be prevented from exploding and crystallizing, and a product with controllable crystal size and good crystallization quality can be obtained. Meanwhile, the continuous crystallization process can reduce the occupied area of equipment, reduce the operation difficulty and reduce the energy consumption.
Disclosure of Invention
Aiming at the technical problems in the prior art, the device is particularly suitable for crystallizing a solid-liquid crystallization system sensitive to temperature and small in metastable zone, and is particularly suitable for the continuous crystallization process for producing aluminum sulfate octadecahydrate.
The circulation continuous crystallizer is characterized in that: comprises a top heating chamber, a middle crystallizing chamber, a bottom crystal collecting chamber, a filtering separator and a mother liquor return pipe, wherein the outer side of the top heating chamber is provided with a heat insulation sleeve; the top heating chamber is provided with a Venturi feeding pipe for introducing a crystal liquid raw material liquid to be treated, a stirring device for stirring the liquid in the top heating chamber and a heating device for heating the liquid in the top heating chamber; a gradient cooling device is arranged on the outer side of the middle crystallization chamber, so that the temperature of the solution in the middle crystallization chamber is reduced in a gradient manner from top to bottom; a flow guide pipe with openings at the upper end and the lower end is fixedly arranged at the center inside the middle crystallization chamber, a plurality of through holes are uniformly formed in the annular wall of the flow guide pipe, and a channel for fluid circulation is formed between the outer side wall of the flow guide pipe and the inner side wall of the middle crystallization chamber; a crystal liquid discharging pipe is arranged at the bottom of the bottom crystal collecting chamber and is connected with the filtering separator through the crystal liquid discharging pipe so as to send a crystal liquid mixture in the bottom crystal collecting chamber into the filtering separator for crystal liquid separation, and a solid outlet of the filtering separator discharges a crystal product after crystal liquid separation; the liquid outlet of the filtering separator is divided into two paths, one path of the liquid outlet discharges mother liquid after crystal liquid separation, the other path of the liquid outlet is connected with one end opening of a mother liquid return pipe, and the other end opening of the mother liquid return pipe penetrates through the bottom crystal collecting chamber and upwards and vertically extends into the guide pipe from the lower end opening of the guide pipe.
The circulation continuous crystallizer is characterized in that: the gradient cooling device comprises N heat exchange interlayers which are arranged outside the middle crystallization chamber at intervals from top to bottom, and a heat exchange medium is respectively introduced into each heat exchange interlayer; from top to bottom, the temperature of the heat exchange media introduced into the N heat exchange interlayers is reduced in sequence; the outer wall of the middle crystallization chamber between two adjacent heat exchange interlayers is provided with a vibrating block; and N is an integer of 5-15.
The circulation continuous crystallizer is characterized in that: the flow guide pipe is of a cylindrical hollow pipe structure or a plurality of regular polygon pipe structures which are sequentially attached and contacted from top to bottom; when the honeycomb duct is a regular polygon tube structure with a plurality of top-down sequentially attached and contacted, the edges and corners of two adjacent regular polygon tubes are arranged in a staggered manner in the vertical direction.
The circulation continuous crystallizer is characterized in that: the top heating chamber comprises a first cylindrical chamber and an inverted conical chamber arranged below the first cylindrical chamber, and the outer sides of the first cylindrical chamber and the inverted conical chamber are coated with the heat insulation sleeves; the length of the draft tube is the same as that of the middle crystallization chamber.
The circulation continuous crystallizer is characterized in that: the stirring device comprises a driving motor, a rotating shaft rod and a stirring blade arranged at the lower end of the rotating shaft rod, the stirring blade is positioned in the center of the inside of the top heating chamber, the middle part of the rotating shaft rod is fixedly arranged at the top of the top heating chamber through a bearing, and the upper end of the rotating shaft rod is fixedly connected with an output shaft of the driving motor; the horizontal interval between the outlet of the Venturi feeding pipe and the rotating shaft rod is smaller than the diameter of the stirring blade, and the rotating shaft rod and the center line of the guide pipe coincide in the vertical direction.
The circulation continuous crystallizer is characterized in that: the heating device comprises a microwave tube, a microwave tube power supply and a microwave protection cover arranged at the top of the top heating chamber, wherein a microwave emitting end of the microwave tube vertically penetrates through the top of the top heating chamber and extends into the top of the top heating chamber, the microwave emitting end of the microwave tube is arranged close to the rotating shaft rod, and the microwave protection cover is arranged right above the microwave tube to prevent microwave leakage.
The circulating continuous crystallizer is characterized in that the bottom crystal collecting chamber comprises a right circular cone chamber and a second cylindrical chamber arranged below the right circular cone chamber, the cooling interlayer is arranged on the outer side of the second cylindrical chamber, and the ratio of the inner diameter of the second cylindrical chamber to the inner diameter of the middle crystallization chamber is 2 ~ 5: 1.
The circulation continuous crystallizer is characterized in that: and the bottom crystal collecting chamber is also provided with a material rake, and crystals deposited at the bottom of the bottom crystal collecting chamber are raked towards the crystal liquid discharging pipe through the material rake and are finally discharged through the crystal liquid discharging pipe.
The circulation continuous crystallizer is characterized in that: the bottom inner wall of the bottom crystal collecting chamber is an inclined plane, the crystal liquid discharging pipe is arranged at the lowest position of the bottom inclined plane of the bottom crystal collecting chamber, and the horizontal inclination angle of the bottom inclined plane of the bottom crystal collecting chamber 3 is 0.3-5 degrees.
Compared with the prior art, the beneficial effect that this application was got is:
the application provides a continuous crystallizer of circulation that comprises top heating chamber, middle part crystallization chamber and bottom crystal collection room for through each part temperature of controlgear, make in the continuous crystallization process, the crystal stays and calms the time length in district, grow into the great crystal of granule (the middle part crystallization chamber outside sets up the gradient heat sink, makes the indoor multistage crystallization condition that exists of middle part crystallization be in the crystallization calm district, and the crystallization process is long in calm district time). Circulation can be formed in the equipment, so that crystallized crystals can be in continuous contact with the reaction liquid mother liquor and have mass transfer, and crystal products with higher purity and quality are obtained. The continuous crystallization process reduces the production intensity, the occupied area of equipment and the unit energy consumption.
Drawings
FIG. 1 is a schematic structural view of a loop continuous crystallizer;
FIG. 2 is a front view of the draft tube when it is a cylindrical hollow tube structure;
FIG. 3 is a top view of the flow guide tube with a plurality of regular polygonal tube structures sequentially contacted from top to bottom;
in the figure: 1-top heating chamber, 101-insulating sleeve, 2-middle crystallizing chamber, 201-guide pipe, 201 a-through hole, 201 b-cylindrical hollow pipe structure, 201 c-regular polygon pipe structure, 202-heat exchange interlayer, 203-vibrating block, 3-bottom crystal collecting chamber, 301-cooling interlayer, 302-material rake, 303-crystal liquid discharging pipe, 4-mother liquid backflow pipe, 5-driving motor, 6-rotating shaft rod, 7-stirring blade, 8-microwave pipe and 9-microwave shield.
Detailed Description
The present invention is further illustrated by the following examples, which should not be construed as limiting the scope of the invention.
Example (b):
a circulation continuous crystallizer comprises a top heating chamber 1, a middle crystallization chamber 2, a bottom crystal collecting chamber 3, a filtering separator and a mother liquor return pipe 4, wherein the outer side of the top heating chamber 1 is provided with a heat insulation sleeve 101; the top heating chamber 1 is provided with a Venturi feeding pipe 101 for introducing a crystal liquid raw material liquid to be treated, a stirring device for stirring the liquid in the top heating chamber and a heating device for heating the liquid in the top heating chamber; a gradient cooling device is arranged on the outer side of the middle crystallization chamber 2, so that the temperature of the solution in the middle crystallization chamber 2 is reduced in a gradient manner from top to bottom; the inside center of the middle crystallization chamber 2 is fixedly provided with a draft tube 201 (compare with fig. 1, the length of the draft tube 201 is the same as the length of the middle crystallization chamber 2, the draft tube 201 is fixedly installed inside the middle crystallization chamber 2 in a way that two opposite sides of the outer wall of the draft tube 201 are fixedly connected with the inner side wall of the middle crystallization chamber 2 through support rods, the fixed connection mode can be welding fixation), the ring wall of the draft tube 201 is uniformly provided with a plurality of through holes 201a, and a channel for fluid circulation is arranged between the outer side wall of the draft tube 201 and the inner side wall of the middle crystallization chamber 2.
A crystal liquid discharging pipe 303 is arranged at the bottom of the bottom crystal collecting chamber 3 and is connected with the filtering separator through the crystal liquid discharging pipe 303 so as to send the crystal liquid mixture in the bottom crystal collecting chamber 3 into the filtering separator for crystal liquid separation, and a solid outlet of the filtering separator discharges crystal products after crystal liquid separation; the liquid outlet of the filtering separator is divided into two paths, one path of the liquid outlet discharges the mother liquid after the crystal liquid separation, the other path of the liquid outlet is connected with one end opening of a mother liquid return pipe 4, the other end opening of the mother liquid return pipe 4 penetrates through the bottom crystal collecting chamber 3, and the mother liquid return pipe extends upwards and vertically into the guide pipe 201 from the lower end opening of the guide pipe 201.
Referring to fig. 1, the top heating chamber 1 includes a first cylindrical chamber and an inverted cone chamber disposed below the first cylindrical chamber, the outer sides of the first cylindrical chamber and the inverted cone chamber are all covered with the insulation cover 101, and the first cylindrical chamber is connected with the upper end of the middle crystallization chamber 2 through the inverted cone chamber.
The stirring device for stirring the liquid in the top heating chamber 1 comprises a driving motor 5, a rotating shaft rod 6 and a stirring blade 7 arranged at the lower end of the rotating shaft rod 6, wherein the stirring blade 7 is positioned in the center of the inside of the top heating chamber 1, the middle part of the rotating shaft rod 6 is fixedly arranged at the top of the top heating chamber 1 through a bearing, and the upper end of the rotating shaft rod 6 is fixedly connected with an output shaft of the driving motor 5; the horizontal distance between the outlet of the venturi feeding pipe 101 and the rotating shaft rod 6 is smaller than the diameter of the stirring blade 7 (the feeding position of the crystal liquid raw material liquid is in the stirring radius range of the stirring device, so that the introduced crystal liquid raw material liquid is stably and uniformly distributed in the top heating chamber 1), and the central lines of the rotating shaft rod 6 and the guide pipe 201 are overlapped in the vertical direction.
The heating device for heating liquid in the top heating chamber 1 comprises a microwave tube 8, a microwave tube power supply and a microwave protection cover 9 arranged at the top of the top heating chamber 1, wherein a microwave emitting end of the microwave tube 8 vertically penetrates through the top of the top heating chamber 1 and extends into the top of the top heating chamber, the microwave emitting end of the microwave tube 8 is close to the rotating shaft rod 6, and the microwave protection cover 9 is arranged right above the microwave tube 8 to prevent microwave leakage. If the crystallization is easily broken by heating with traditional electric heating rod or heating coil, because of the temperature gradient in the convection heat transfer process, the crystallization is easy to be carried out quickly and stably.
In the device of this application, when heating top heating chamber 1 inside liquid through microwave tube power drive microwave pipe 8 transmission microwave, the liquid in top heating chamber 1 is through absorbing the microwave that drives microwave pipe 8 transmission and rise temperature, and this process is not only heating energy consumption low, owing to adopt radiation heat transfer rather than convection heat transfer, the microwave emission end of microwave pipe 8 and the interior liquid temperature difference of top heater are little, consequently be difficult for taking place the phenomenon of quick, a large amount of crystallization scaling. The connection among the top heating chamber 1, the middle crystallizing chamber 2 and the bottom crystal collecting chamber 3 is basically a closed structure, the microwave emitted by the driving microwave tube 8 basically has no leakage, but the connection between the microwave tube 8 and the top of the top heating chamber 1 is not closed well, so the microwave shield 9 is designed to further improve the safety of the equipment operation.
The gradient cooling device arranged outside the middle crystallization chamber 2 comprises N heat exchange interlayers 202 (N is an integer of 5-15) which are arranged outside the middle crystallization chamber 2 from top to bottom at intervals, and heat exchange media are respectively introduced into each heat exchange interlayer 202; from top to bottom, the temperature of the heat exchange media introduced into the N heat exchange interlayers 202 is reduced in sequence; and the outer walls of the middle crystallization chambers 2 between two adjacent heat exchange interlayers 202 are provided with vibrating blocks 203. When the device of this application is used for carrying out crystallization treatment to crystal liquid raw materials liquid, the temperature of liquid is a little higher than the heat transfer medium temperature that lets in the topmost heat transfer intermediate layer 202 in the middle part crystallization chamber 2 outside in top heating chamber 1.
The crystal growth is realized to the liquid crystal raw materials liquid basically in the passageway between honeycomb duct 201 outside lateral wall and the inside lateral wall of middle part crystallization chamber 2, and the device of this application is in order to improve the crystallization effect at the practical application in-process: the temperature change of the heat exchange media in the N-2 heat exchange interlayers 202 is small, so that the crystallization process is in a metastable zone for a long time, crystal nuclei can effectively grow, and crystals with large particles are formed; and the temperature change of the heat exchange medium in the 2 heat exchange interlayers 202 at the bottom is large, so that the sedimentation of the crystals is completed. The purpose in which the vibrating mass 203 is arranged is: the outer wall of the middle crystallization chamber 2 is vibrated by the vibrating mass 203, and the crystals are prevented from scaling on the inner wall of the middle crystallization chamber 2.
When the device of the application carries out crystallization treatment on the crystal liquid raw material liquid, after the crystal liquid mixture discharged from the crystal liquid discharging pipe 303 is subjected to crystal liquid separation in the filtering separator, the obtained mother liquid part is forced to flow back into the guide pipe 201, so that the liquid inside the guide pipe moves along the guide pipe from bottom to top, the liquid-solid mixture outside the guide pipe moves from top to bottom, circulation is formed inside and outside the guide pipe 201, and under the existence of the through holes 201a on the annular wall of the guide pipe 201, the substances inside and outside the guide pipe 201 can be in continuous contact and mass transfer, and the purity and the quality of a crystallized product are improved.
Referring to fig. 2 and fig. 3, the flow guide pipe 201 is a cylindrical hollow pipe structure 201b (two opposite sides of the cylindrical hollow pipe structure 201b are provided with a support rod), or is a plurality of regular polygon pipe structures 201c sequentially attached and contacted from top to bottom; when the honeycomb duct 201 is a regular polygon tube structure with a plurality of top-down sequentially attached and contacted, edges and corners of two adjacent regular polygon tubes are arranged in a staggered mode in the vertical direction (the regular polygon tubes are simple to process and are arranged in a staggered mode to prevent liquid from flowing in the honeycomb duct 201 to form dead angles), and the outer wall of each regular polygon tube can be fixedly connected with the inner wall of the middle crystallization chamber 2 through a support rod.
Referring to fig. 1, the bottom crystal collecting chamber 3 comprises a right circular cone chamber and a second cylindrical chamber disposed below the right circular cone chamber, the second cylindrical chamber is communicated with the lower end of the middle crystallization chamber 2 through the right circular cone chamber, the cooling interlayer 301 is disposed outside the second cylindrical chamber, and the ratio of the inner diameter of the second cylindrical chamber to the inner diameter of the middle crystallization chamber 2 is 2 ~ 5: 1.
And a material rake 302 is further arranged on the bottom crystal collecting chamber 3, and crystals deposited at the bottom of the bottom crystal collecting chamber 3 are raked towards a crystal liquid discharge pipe 303 through the material rake 302 and are finally discharged through the crystal liquid discharge pipe 303. The bottom inner wall of the bottom crystal collection chamber 3 is an inclined plane, the crystal liquid discharge pipe 303 is arranged at the lowest position of the bottom inclined plane of the bottom crystal collection chamber 3, and the horizontal inclination angle of the bottom inclined plane of the bottom crystal collection chamber 3 is 0.3-5 degrees. The formed crystals can be enriched near the crystal liquid discharge pipe 303 under the action of gravity and mechanical force raked by the material raking 302 and are finally conveyed out of the bottom crystal collecting chamber 3.
The circulation continuous crystallizer is suitable for a solid-liquid two-phase crystallization system with solid density larger than liquid density, the liquid-solid ratio of reaction liquid mother liquid to crystals which is suitable for operation is 0.5 ~ 5: 1, the solid content in the middle crystallization chamber 2 of the circulation continuous crystallizer is gradually increased from top to bottom, in order to ensure that the crystallizer can continuously operate, the ratio of the inner diameter of a second cylindrical chamber of a bottom crystal collecting chamber 3 to the inner diameter of the middle crystallization chamber 2 is 2 ~ 5: 1, the reaction liquid mother liquid and the crystals are forcibly refluxed into a draft tube 201 through the mother liquid part, the liquid-solid ratio of the reaction liquid mother liquid to the crystals is adjusted, and the possibility that the device is blocked by crystal deposition is reduced.
Example 1:
when the circulation continuous crystallizer is used for treating the raw material liquid of the crystal liquid, the process is as follows:
the raw material liquid of the crystal liquid is fed by adopting an aluminum sulfate aqueous solution with the aluminum sulfate mass concentration of 59.2% and the temperature of the raw material liquid of the crystal liquid in the top heating chamber 1 is controlled to be 95 ℃ by microwave heating.
The outer side of the middle crystallization chamber 2 is provided with 7 heat exchange interlayers 202 from top to bottom at intervals, the temperature of the fluid introduced into the upper five heat exchange interlayers 202 is 94.5 ℃, 94 ℃, 93 ℃, 92 ℃ and 90 ℃ in sequence, and the temperature of the fluid introduced into the lowest two heat exchange interlayers 202 is 75 ℃ and 40 ℃ in sequence. And (3) introducing a cooling fluid into a cooling interlayer 301 outside the bottom crystal collection chamber 3, controlling the temperature of a crystal liquid mixture in the bottom crystal collection chamber 3 to be about 25 ℃, and controlling the liquid-solid ratio of a mother liquid to aluminum sulfate crystals in the crystal liquid mixture in the bottom crystal collection chamber 3 in a mother liquid reflux mode to be 3: about 1.
And (3) feeding the crystal liquid mixture in the bottom crystal collection chamber 3 into a filtering separator for crystal liquid separation to obtain aluminum sulfate crystals and mother liquid, and washing and drying the obtained aluminum sulfate crystals by using a saturated aluminum sulfate aqueous solution to obtain an aluminum sulfate product. The quality of the obtained aluminum sulfate product is detected, and the result is as follows:
aluminum sulfate product: 17.15% Al2O30.08% of insoluble matter in water, 92.4% of whiteness, and 2.3mm of average particle size. When the prepared aluminum sulfate product is dissolved in water to prepare an aqueous solution with the mass concentration of 1%, the pH value = 3.7.
The statements in this specification merely set forth a list of implementations of the inventive concept and the scope of the present invention should not be construed as limited to the particular forms set forth in the examples.
Claims (9)
1. A circulation continuous crystallizer is characterized in that: comprises a top heating chamber (1) with a heat insulation sleeve (101) arranged on the outer side, a middle crystallization chamber (2), a bottom crystal collecting chamber (3) with a cooling interlayer (301) arranged on the outer side, a filtering separator and a mother liquid return pipe (4); the top heating chamber (1) is provided with a Venturi feed pipe (101) for introducing a crystal liquid raw material liquid to be treated, a stirring device for stirring the liquid in the top heating chamber and a heating device for heating the liquid in the top heating chamber; a gradient cooling device is arranged on the outer side of the middle crystallization chamber (2) so that the temperature of the solution in the middle crystallization chamber (2) is reduced in a gradient manner from top to bottom; a flow guide pipe (201) with openings at the upper end and the lower end is fixedly arranged at the center inside the middle crystallization chamber (2), a plurality of through holes (201 a) are uniformly formed in the annular wall of the flow guide pipe (201), and a channel for fluid circulation is formed between the outer side wall of the flow guide pipe (201) and the inner side wall of the middle crystallization chamber (2);
a crystal liquid discharging pipe (303) is arranged at the bottom of the bottom crystal collecting chamber (3) and is connected with the filtering separator through the crystal liquid discharging pipe (303) so as to send a crystal liquid mixture in the bottom crystal collecting chamber (3) into the filtering separator for crystal liquid separation, and a solid outlet of the filtering separator discharges a crystal product after crystal liquid separation; the liquid outlet of the filtering separator is divided into two paths, one path of liquid outlet discharges mother liquid after crystal liquid separation, the other path of liquid outlet is connected with an opening at one end of a mother liquid return pipe (4), an opening at the other end of the mother liquid return pipe (4) penetrates through the bottom crystal collecting chamber (3) and upwards and vertically extends into the guide pipe (201) from an opening at the lower end of the guide pipe (201).
2. A continuous loop crystallizer as claimed in claim 1, wherein: the gradient cooling device comprises N heat exchange interlayers (202) which are arranged at the outer side of the middle crystallization chamber (2) from top to bottom at intervals, and a heat exchange medium is respectively introduced into each heat exchange interlayer (202); from top to bottom, the temperature of the heat exchange media introduced into the N heat exchange interlayers (202) is reduced in sequence; the outer wall of the middle crystallization chamber (2) between two adjacent heat exchange interlayers (202) is provided with a vibration block (203); and N is an integer of 5-15.
3. A continuous loop crystallizer as claimed in claim 1, wherein: the honeycomb duct (201) is of a cylindrical hollow tube structure or a plurality of regular polygon tube structures which are sequentially attached and contacted from top to bottom; when the honeycomb duct (201) is a regular polygon tube structure with a plurality of top-down sequentially attached and contacted, the edges and corners of two adjacent regular polygon tubes are arranged in a staggered mode in the vertical direction.
4. A continuous loop crystallizer as claimed in claim 1, wherein: the top heating chamber (1) comprises a first cylindrical chamber and an inverted conical chamber arranged below the first cylindrical chamber, and the outer sides of the first cylindrical chamber and the inverted conical chamber are coated with the heat-insulating sleeve (101); the length of the draft tube (201) is the same as that of the middle crystallization chamber (2).
5. A continuous loop crystallizer as claimed in claim 1, wherein: the stirring device comprises a driving motor (5), a rotating shaft rod (6) and a stirring blade (7) arranged at the lower end of the rotating shaft rod (6), the stirring blade (7) is positioned in the center of the inside of the top heating chamber (1), the middle part of the rotating shaft rod (6) is fixedly arranged at the top of the top heating chamber (1) through a bearing, and the upper end of the rotating shaft rod (6) is fixedly connected with an output shaft of the driving motor (5); the horizontal distance between the outlet of the Venturi feeding pipe (101) and the rotating shaft rod (6) is smaller than the diameter of the stirring blade (7), and the rotating shaft rod (6) and the center line of the guide pipe (201) coincide in the vertical direction.
6. A continuous crystallizer for recirculating streams as set forth in claim 5, wherein: the heating device comprises a microwave tube (8), a microwave tube power supply and a microwave protection cover (9) arranged at the top of the top heating chamber (1), wherein the microwave emitting end of the microwave tube (8) vertically penetrates through the top of the top heating chamber (1) and extends into the top of the top heating chamber, the microwave emitting end of the microwave tube (8) is close to the rotating shaft rod (6) and arranged, and the microwave protection cover (9) is arranged right above the microwave tube (8) to prevent microwave leakage.
7. The continuous circulating crystallizer as claimed in claim 1, wherein the bottom crystal collecting chamber (3) comprises a right circular cone chamber and a second cylindrical chamber arranged below the right circular cone chamber, the cooling jacket (301) is arranged outside the second cylindrical chamber, and the ratio of the inner diameter of the second cylindrical chamber to the inner diameter of the middle crystallizing chamber (2) is 2 ~ 5: 1.
8. A continuous loop crystallizer as claimed in claim 1, wherein: and the bottom crystal collecting chamber (3) is also provided with a material rake (302), and crystals deposited at the bottom of the bottom crystal collecting chamber (3) are raked towards the crystal liquid discharging pipe (303) through the material rake (302) and are finally discharged through the crystal liquid discharging pipe (303).
9. The continuous loop crystallizer of claim 8, wherein: the bottom inner wall of the bottom crystal collecting chamber (3) is an inclined plane, the crystal liquid discharging pipe (303) is arranged at the lowest position of the bottom inclined plane of the bottom crystal collecting chamber (3), and the horizontal inclination angle of the bottom inclined plane of the bottom crystal collecting chamber (3) is 0.3-5 degrees.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910955126.7A CN110585757B (en) | 2019-10-09 | 2019-10-09 | Circulation continuous crystallizer |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201910955126.7A CN110585757B (en) | 2019-10-09 | 2019-10-09 | Circulation continuous crystallizer |
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| CN110585757A true CN110585757A (en) | 2019-12-20 |
| CN110585757B CN110585757B (en) | 2024-07-02 |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
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| CN110585757B (en) | 2024-07-02 |
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