CN115304081B - Preparation method and device of electronic-grade potassium hydroxide - Google Patents
Preparation method and device of electronic-grade potassium hydroxide Download PDFInfo
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- CN115304081B CN115304081B CN202211113167.XA CN202211113167A CN115304081B CN 115304081 B CN115304081 B CN 115304081B CN 202211113167 A CN202211113167 A CN 202211113167A CN 115304081 B CN115304081 B CN 115304081B
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract description 255
- 238000002360 preparation method Methods 0.000 title claims abstract description 16
- 238000001816 cooling Methods 0.000 claims abstract description 187
- 239000013078 crystal Substances 0.000 claims abstract description 23
- 239000000498 cooling water Substances 0.000 claims abstract description 16
- 238000011282 treatment Methods 0.000 claims abstract description 14
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 12
- 239000011259 mixed solution Substances 0.000 claims abstract description 11
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 238000000034 method Methods 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims abstract description 6
- 238000000926 separation method Methods 0.000 claims abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims description 27
- 230000008859 change Effects 0.000 claims description 23
- 238000007789 sealing Methods 0.000 claims description 12
- 230000007246 mechanism Effects 0.000 claims description 11
- 238000005192 partition Methods 0.000 claims description 10
- 238000007790 scraping Methods 0.000 claims description 10
- 235000017166 Bambusa arundinacea Nutrition 0.000 claims description 9
- 235000017491 Bambusa tulda Nutrition 0.000 claims description 9
- 241001330002 Bambuseae Species 0.000 claims description 9
- 235000015334 Phyllostachys viridis Nutrition 0.000 claims description 9
- 239000011425 bamboo Substances 0.000 claims description 9
- 238000000227 grinding Methods 0.000 claims description 4
- 239000002994 raw material Substances 0.000 claims description 4
- 230000005540 biological transmission Effects 0.000 claims description 3
- 238000002425 crystallisation Methods 0.000 abstract description 7
- 230000008025 crystallization Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 1
- 238000005457 optimization Methods 0.000 description 7
- 238000010586 diagram Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000003756 stirring Methods 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007599 discharging Methods 0.000 description 1
- 238000007580 dry-mixing Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001914 filtration Methods 0.000 description 1
- 230000008014 freezing Effects 0.000 description 1
- 238000007710 freezing Methods 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009434 installation Methods 0.000 description 1
- 238000005342 ion exchange Methods 0.000 description 1
- 230000000750 progressive effect Effects 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910001415 sodium ion Inorganic materials 0.000 description 1
- 125000006850 spacer group Chemical group 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01D—SEPARATION
- B01D9/00—Crystallisation
- B01D9/0004—Crystallisation cooling by heat exchange
-
- 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
- B01D9/02—Crystallisation from solutions
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F27/00—Mixers with rotary stirring devices in fixed receptacles; Kneaders
- B01F27/60—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis
- B01F27/70—Mixers with rotary stirring devices in fixed receptacles; Kneaders with stirrers rotating about a horizontal or inclined axis with paddles, blades or arms
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/10—Maintenance of mixers
- B01F35/12—Maintenance of mixers using mechanical means
- B01F35/123—Maintenance of mixers using mechanical means using scrapers for cleaning mixers
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F35/93—Heating or cooling systems arranged inside the receptacle
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D1/00—Oxides or hydroxides of sodium, potassium or alkali metals in general
- C01D1/04—Hydroxides
- C01D1/28—Purification; Separation
- C01D1/30—Purification; Separation by crystallisation
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
- B01F35/00—Accessories for mixers; Auxiliary operations or auxiliary devices; Parts or details of general application
- B01F35/90—Heating or cooling systems
- B01F2035/98—Cooling
Landscapes
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Organic Chemistry (AREA)
- Engineering & Computer Science (AREA)
- Crystallography & Structural Chemistry (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Mechanical Engineering (AREA)
- Physics & Mathematics (AREA)
- Thermal Sciences (AREA)
- Heat-Exchange Devices With Radiators And Conduit Assemblies (AREA)
Abstract
The invention relates to a preparation method and a device of electronic-grade potassium hydroxide, comprising the following steps: introducing a 25% -30% low-concentration solution product prepared from industrial-grade potassium hydroxide into evaporation equipment, and evaporating and concentrating the 25% -30% potassium hydroxide solution to 50% -55% potassium hydroxide saturated solution through evaporation and concentration; cooling water at 7-12 ℃ is introduced into the crystallizer, and then 50% -55% potassium hydroxide saturated solution is introduced into the crystallizer for cooling treatment, so that the solubility of potassium hydroxide in the potassium hydroxide saturated solution is reduced; cooling the crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and then introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation; adding pure water into potassium hydroxide crystals separated by a disc centrifuge for dissolution to obtain electronic-grade potassium hydroxide solution; the method has the advantages of simple steps, high cooling efficiency of the crystallizer and good crystallization effect of the potassium hydroxide solution.
Description
Technical Field
The invention belongs to the technical field of potassium hydroxide preparation, and particularly relates to a preparation method and device of electronic-grade potassium hydroxide.
Background
With the development of the domestic market demands and the semiconductor and electronic industries, the requirements of customers on the quality of potassium hydroxide solution are higher and higher, the requirements of industrial-grade potassium hydroxide are not met, and the industrial-grade potassium hydroxide is required to be purified, so that the quality is improved; at present, the electronic grade potassium hydroxide is generally produced by preparing potassium hydroxide into potassium hydroxide solution, then removing heavy metals and sodium ions by adopting methods such as ion exchange or cooling, freezing and crystallization, and the like.
Disclosure of Invention
The purpose of the invention is that: aims to provide a preparation method and a preparation device of electronic-grade potassium hydroxide, which are used for solving the problems in the background technology.
In order to achieve the technical purpose, the invention adopts the following technical scheme:
the preparation method of the electronic grade potassium hydroxide comprises the following steps:
s1, introducing a 25% -30% low-concentration solution product prepared from industrial-grade potassium hydroxide into evaporation equipment, and evaporating and concentrating a 25% -30% potassium hydroxide solution to a 50% -55% potassium hydroxide saturated solution through evaporation and concentration;
s2, introducing 7-12 ℃ cooling water into the crystallizer, and then introducing 50-55% potassium hydroxide saturated solution into the crystallizer for cooling treatment, so that the solubility of potassium hydroxide in the potassium hydroxide saturated solution is reduced;
s3, cooling the mixed solution by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and then introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
s4, adding pure water into the potassium hydroxide crystals separated by the disc type centrifugal machine to dissolve the potassium hydroxide crystals, and obtaining the electronic-grade potassium hydroxide solution.
The utility model provides a preparation facilities of electronic grade potassium hydroxide, is applied to step S2 of preparation facilities of electronic grade potassium hydroxide, includes base, cooling storehouse and closing cap, the cooling storehouse assemble in the base upper end, the closing cap seals and locates cooling storehouse upper end, feed inlet and discharge gate have been seted up respectively to both ends around the cooling storehouse upside, cooling storehouse inboard is equipped with cooling mechanism, cooling mechanism includes a plurality of cooling plates, a plurality of the cooling plate evenly assemble in cooling storehouse inboard, a plurality of the cooling tank has all been seted up to the cooling plate inboard, cooling plate upper portion left and right sides all be equipped with the connecting pipe that the cooling tank is linked together, cooling storehouse both sides are fixed and are equipped with a plurality of cooling pipes, the cooling pipe with fixed connection can be dismantled to the connecting pipe.
Preferably, the cooling bin is further provided with a mixing mechanism, the mixing mechanism comprises a driving motor, a main shaft and a plurality of mixing components, the driving motor is fixedly assembled at the upper end of the base, the main shaft is rotationally arranged at the inner side of the cooling bin, one end of the main shaft is sealed and rotationally penetrated through the cooling bin and is connected with the driving motor in a transmission manner, the mixing components are uniformly assembled in the cooling bin, the mixing components are respectively positioned between two adjacent cooling plates, the mixing components are fixedly assembled at the main shaft, the cooling plates are matched with the inner side of the cooling bin in shape, and the lower side of the cooling plate is provided with a notch.
Preferably, the blending assembly comprises two semicircular plates, the two opposite ends of the semicircular plates are jointly provided with mounting rings matched with the main shaft, a plurality of partition plates are arranged on the front side and the rear side of each semicircular plate, each partition plate is provided with a mounting hole, a plurality of mounting holes are respectively provided with bolts and nuts, the bottom of the cooling bin is semicircular, and the two semicircular plates are matched with the bottom of the cooling bin in shape.
Preferably, the cooling plate is further provided with a scraping assembly on the inner side, the scraping assembly comprises a first rotating ring, a second rotating ring, a torsion spring, a base, a stepped boss, a spring, a clamping table, a gradual change ring and a scraping plate, a rotating groove is formed in the middle of the cooling plate, the first rotating ring is rotationally sealed to be arranged in the rotating groove, a main shaft is fixedly connected with the inner side of the first rotating ring, the second rotating ring is rotationally sealed to be arranged in the cooling groove, the first rotating ring is positioned on the inner side of the second rotating ring, the torsion spring is assembled between the first rotating ring and the second rotating ring, one end of the torsion spring is fixedly connected with the inner wall of the cooling plate, the other end of the torsion spring is fixedly connected with the inner side of the second rotating ring, the base is fixedly arranged on the outer side of the first rotating ring, the step groove is formed in a sliding manner, one end of the stepped boss is fixedly arranged in the inner side of the step groove, the spring is fixedly assembled between the boss and the step groove, the clamping table is fixedly arranged on the inner side of the second rotating ring, the gradual change ring is assembled between the first rotating ring and the inner side of the cooling plate, the gradual change ring is gradually connected with the inner side of the cooling plate, and the gradual change ring is gradually connected with the inner side of the cooling plate.
Preferably, the number of the scrapers is at least two, a plurality of scrapers are arranged on the outer side of the second rotating ring, the scrapers on the lower left side are close to the inner wall of the cooling plate, the scrapers are not arranged on the lower right side in the cooling tank, the included angle between two adjacent scrapers is the same as the included angle between the right-most scrapers and the inner wall of the lower right corner of the cooling plate, and the shape of each scraper is an annular strip.
Preferably, an L-shaped ring plate matched with the torsion spring is fixedly arranged on the inner side of the second rotating ring.
Preferably, the connecting pipe outside rotates the cover and is equipped with the screw thread section of thick bamboo, the screw thread section of thick bamboo with cooling tube threaded connection, the screw thread section of thick bamboo with be equipped with the raw material area between the cooling tube, the connecting pipe outside with the screw thread section of thick bamboo inboard all is equipped with mutually supporting sealing ring.
Preferably, a plurality of treatment areas are arranged on the front side and the rear side of the cooling plate, and grinding thinning treatment is carried out on the treatment areas.
The invention has the following benefits: after the potassium hydroxide solution enters the cooling bin, the potassium hydroxide solution can sequentially pass through the cooling plates and the semicircular plates which are arranged in a staggered manner, a plurality of rotating semicircular plates can stir and mix the potassium hydroxide solution passing through the cooling bin uniformly, meanwhile, the surfaces of the cooling plates can be scraped, separated crystals are prevented from being close to the cooling plates, the cooling efficiency is improved, the semicircular plates are close to the cooling plates, the potassium hydroxide solution can be driven to circulate and transport in the cooling bin, the moving path of the potassium hydroxide solution is increased, the heat exchange time between the potassium hydroxide solution and the cooling plates is prolonged, and the crystallization efficiency is improved; through the scraper blade that sets up in the cooling plate inboard, can follow main shaft circulation and rotate, strike off the inside dirt of cooling plate, reciprocating scraper blade that scrapes can also make dirt and cooling water mixing, makes its inside of discharging cooling plate, avoids the cooling water scale deposit, makes heat exchange efficiency improve.
Drawings
The invention may be further illustrated by means of non-limiting examples given in the accompanying drawings.
FIG. 1 is a schematic diagram of an apparatus for preparing electronic grade potassium hydroxide according to an embodiment of the present invention;
FIG. 2 is a schematic view showing a partial structure of a first embodiment of an apparatus for preparing electronic grade potassium hydroxide according to the present invention;
FIG. 3 is a schematic view showing a partial sectional structure of a first embodiment of an apparatus for preparing electronic grade potassium hydroxide according to the present invention;
FIG. 4 is an enlarged schematic view of FIG. 3 at A;
FIG. 5 is a schematic view showing a partial sectional structure of a second embodiment of an apparatus for preparing electronic grade potassium hydroxide according to the present invention;
FIG. 6 is an enlarged schematic view at B in FIG. 5;
FIG. 7 is a schematic view showing the structure of a cooling plate in a third embodiment of an apparatus for preparing electronic grade potassium hydroxide according to the present invention;
FIG. 8 is a schematic diagram showing a cross-sectional structure of a cooling plate in a third embodiment of an apparatus for producing electronic grade potassium hydroxide according to the present invention;
FIG. 9 is a schematic diagram showing a cross-sectional structure of a cooling plate in a third embodiment of an apparatus for producing electronic grade potassium hydroxide according to the present invention;
FIG. 10 is an enlarged schematic view of FIG. 9C;
FIG. 11 is a schematic diagram showing a cross-sectional structure of a cooling plate in a third embodiment of an apparatus for producing electronic grade potassium hydroxide according to the present invention;
FIG. 12 is an enlarged schematic view of FIG. 11 at D;
the main reference numerals are as follows:
base 1, cooling bin 11, closing cap 111, feed inlet 112, discharge outlet 113, cooling plate 12, cooling tank 121, connecting tube 122, cooling tube 123, notch 124, screw cylinder 125, sealing ring 126, treatment area 127, driving motor 13, spindle 14, semicircular plate 15, mounting ring 151, spacer 152, first rotating ring 21, rotating tank 211, second rotating ring 22, torsion spring 23, L-shaped ring plate 231, base 24, stepped boss 241, spring 242, stepped tank 243, clamping table 25, progressive ring 26, scraper 27.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following technical scheme of the present invention will be further described with reference to the accompanying drawings and examples.
The invention relates to a preparation method of electronic grade potassium hydroxide, which comprises the following steps:
s1, introducing a 25% -30% low-concentration solution product prepared from industrial-grade potassium hydroxide into evaporation equipment, and evaporating and concentrating a 25% -30% potassium hydroxide solution to a 50% -55% potassium hydroxide saturated solution through evaporation and concentration;
s2, introducing 7-12 ℃ cooling water into the crystallizer, and then introducing 50-55% potassium hydroxide saturated solution into the crystallizer for cooling treatment, so that the solubility of potassium hydroxide in the potassium hydroxide saturated solution is reduced;
s3, cooling the mixed solution by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and then introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
s4, adding pure water into the potassium hydroxide crystals separated by the disc type centrifugal machine to dissolve the potassium hydroxide crystals, and obtaining the electronic-grade potassium hydroxide solution.
Embodiment one:
as shown in fig. 1-4, the preparation device of electronic grade potassium hydroxide of the present invention is applied to step S2 of the preparation method of electronic grade potassium hydroxide, and comprises a base 1, a cooling bin 11 and a sealing cover 111, wherein the cooling bin 11 is assembled at the upper end of the base 1, the sealing cover 111 is arranged at the upper end of the cooling bin 11 in a sealing manner, a feed inlet 112 and a discharge outlet 113 are respectively arranged at the front end and the rear end of the upper side of the cooling bin 11, a cooling mechanism is arranged at the inner side of the cooling bin 11, the cooling mechanism comprises a plurality of cooling plates 12, the cooling plates 12 are uniformly assembled at the inner side of the cooling bin 11, cooling grooves 121 are respectively arranged at the inner sides of the cooling plates 12, connecting pipes 122 communicated with the cooling grooves 121 are respectively arranged at the left side and the right side of the upper part of the cooling plates 12, a plurality of cooling pipes 123 are fixedly arranged at the two sides of the cooling bin 11, and the cooling pipes 123 are detachably and fixedly connected with the connecting pipes 122.
The cooling bin 11 is further provided with a mixing mechanism, the mixing mechanism comprises a driving motor 13, a main shaft 14 and a plurality of mixing components, the driving motor 13 is fixedly assembled at the upper end of the base 1, the main shaft 14 is rotationally arranged on the inner side of the cooling bin 11, one end of the main shaft 14 is in sealed rotation to penetrate through the cooling bin 11 and is in transmission connection with the driving motor 13, the mixing components are uniformly assembled inside the cooling bin 11 and are respectively positioned between two adjacent cooling plates 12, the mixing components are fixedly assembled on the main shaft 14, the cooling plates 12 are matched with the inner side of the cooling bin 11 in shape, and the lower side of each cooling plate 12 is provided with a notch 124.
The mixing components and the cooling plates 12 in the cooling bin 11 are distributed in a staggered manner, and the mixing components close to the feed inlet 112 and the discharge outlet 112 can stir the in-out solution; the cooling pipes 123 on the left and right sides are used for externally connecting an output device and a recovery device of cooling water, which are conventional technical means; when the device is used for crystallizing potassium hydroxide solution, the potassium hydroxide solution is introduced from the feed inlet 112 of the cooling bin 11, cooling water is continuously introduced into the cooling grooves 121 of the cooling plates 12 through the cooling pipes 123, the cooling water enters from the connecting pipe 122 on one side of the cooling plates 12 and flows out from the connecting pipe 122 on the other side of the cooling plates 12, the potassium hydroxide solution sequentially passes through the notches 124 of the cooling plates 12 to flow towards the discharge outlet 113 after entering the cooling bin 11, and in the process, the mixing components are driven to rotate by the driving motor 13, and the mixing components slowly rotate to mix and stir the potassium hydroxide solution in heat exchange, so that the potassium hydroxide solution is uniformly heat exchanged, the heat exchange efficiency is improved, and the crystallization efficiency is increased.
As shown in fig. 4, in the optimization of this embodiment, a threaded cylinder 125 is rotatably sleeved on the outer side of the connecting pipe 122, the threaded cylinder 125 is in threaded connection with the cooling pipe 123, a raw material belt is assembled between the threaded cylinder 125 and the cooling pipe 123, and sealing rings 126 matched with each other are respectively arranged on the outer side of the connecting pipe 122 and the inner side of the threaded cylinder 125.
The raw material area can increase the leakproofness of threaded connection department, lasts the screw thread through both sides screw thread section of thick bamboo 125 and rotates the cover and locate cooling tube 123, can make two sealing ring 126 subassembly be close to this carry out sealing treatment through two sealing rings 126 to the connection, the operating personnel of being convenient for communicates connecting pipe 122 and cooling tube 123, the installation of being convenient for.
As shown in fig. 3, in the optimization of this embodiment, the front and rear sides of the cooling plate 12 are provided with a plurality of processing areas 127, and the plurality of processing areas 127 are subjected to grinding and thinning processing.
The outside of the cooling plate 12 is subjected to a plurality of grinding thinning treatments, so that the thickness of the cooling plate 12 in a partial area can be reduced, the part is more beneficial to heat conduction, cooling water heat exchange and the crystallization efficiency of potassium hydroxide solution is improved.
Embodiment two:
as shown in fig. 5-6, for further optimization of the first embodiment, the mixing component includes two semicircular plates 15, opposite ends of the two semicircular plates 15 are provided with mounting rings 151 matched with the main shaft 14, two sides of the two semicircular plates 15 are provided with a plurality of partition plates 152, two adjacent partition plates 152 on the two semicircular plates 15 are provided with mounting holes, the mounting holes are provided with bolts and nuts, the bottom of the cooling bin 11 is semicircular, and the two semicircular plates 15 are matched with the bottom of the cooling bin 11 in shape.
The two semicircular plates 15 can be fixedly installed together through a plurality of mounting holes and by means of bolts and nuts, and at the moment, the two mounting rings 151 can be fixedly clamped on the main shaft 14, so that the driving motor 13 is started to drive the dry mixing components to rotate; because the two semicircular plates 15 are matched with the bottom of the cooling bin 11 in shape, and the front side and the rear side of the two semicircular plates 15 are provided with the plurality of partition plates 152, the plurality of partition plates 152 isolate the semicircular plates 15 into a plurality of sector areas, after the potassium hydroxide solution is introduced into the cooling bin 11, the potassium hydroxide solution does not slightly pass through the mixing component from the lower side, the area isolated by the plurality of partition plates 152 rotates, when the semicircular plates 15 rotate to the upper side, the potassium hydroxide solution at the upper side enters the other side of the semicircular plates 15 from the side, then continues to rotate along the semicircular plates 15 until the semicircular plates rotate to the lower side, the potassium hydroxide solution passes through the notch 124 of the cooling plate 12 and flows into one side of the next semicircular plate 15, and the potassium hydroxide solution circulates in sequence, so that the flow path of the potassium hydroxide solution can be increased, and the potassium hydroxide solution can fully contact with the cooling plate 12 to perform heat exchange, and the heat exchange effect is improved;
when a plurality of cooling plates 12 exchange heat, the phenomenon that crystals are precipitated can appear in the position that is close to the cooling plates 12, and the precipitated crystals can be pressed close to the cooling plates, so that the efficiency of heat exchange between potassium hydroxide solution and the cooling plates 12 can be reduced, and therefore, only the semicircular plates 15 are required to be installed close to the cooling plates 12 when the semicircular plates 15 are installed, and when the uniformly-mixed components are slowly stirred and uniformly mixed, the surfaces of the cooling plates 12 can be scraped and cleaned, the precipitated crystals are prevented from being pressed close to the side edges of the cooling plates 12, and the efficiency of cooling and heat exchange is improved.
Embodiment III:
as shown in fig. 7-12, for further optimization of the first embodiment, and simultaneous optimization and improvement of the second embodiment, a scraping assembly is further provided on the inner side of the cooling plate 12, the scraping assembly includes a first rotating ring 21, a second rotating ring 22, a torsion spring 23, a base 24, a stepped boss 241, a spring 242, a clamping table 25, a gradual change ring 26, and a scraper 27, a rotating groove 211 is provided in the middle of the cooling plate 12, the first rotating ring 21 is rotationally sealed in the rotating groove 211, the main shaft 14 is fixedly connected with the inner side of the first rotating ring 21, the second rotating ring is rotationally sealed in the cooling groove 121, the first rotating ring 21 is located on the inner side of the second rotating ring 22, the torsion spring 23 is assembled between the first rotating ring 21 and the second rotating ring 22, one end of the torsion spring 23 is fixedly connected with the inner wall of the cooling plate 12, the other end of the torsion spring 23 is fixedly connected with the inner side of the second rotating ring 22, the base 24 is fixedly arranged on the outer side of the first rotating ring 21, the base 24 is provided with a stepped groove 243, one end of a stepped boss 241 is slidably arranged in the stepped groove 243, a spring 242 is fixedly assembled between the stepped boss 241 and the stepped groove 243, a clamping table 25 is fixedly arranged on the inner side of the second rotating ring 22, a gradual change ring 26 is assembled between the first rotating ring 21 and the second rotating ring 22, the gradual change ring 26 is fixedly connected with the inner wall of the cooling plate 12, the gradual change ring 26 is an unsealed ring, the inner side of one end of the gradual change ring 26 gradually gathers towards the end, the gradual change ring 26 and the clamping table 25 are staggered, the stepped boss 241 is matched with the gradual change ring 26 and the clamping table 25, and the scraping plate 27 is fixedly arranged on the outer side of the second rotating ring 22.
Because cooling water is introduced into the cooling tank 121 of the cooling plate 12 for a long time to exchange heat with the potassium hydroxide solution, the cooling tank 121 filled with the cooling water can be scaled, dirt can adhere to the inside of the cooling tank 121, so that the crystallization efficiency of the potassium hydroxide solution can be seriously reduced, and the descaling treatment of the cooling plate 12 is quite troublesome, so that the cooling plate 12 is optimized and improved;
by the dynamic seal mounting of the first rotating ring 21 and the second rotating ring 22, the parts between the first rotating ring 21 and the second rotating ring 22 can be protected; one end of the torsion spring 23 is fixedly connected with the second rotating ring 22, and the other end is fixedly connected with the inside of the cooling groove 121, so that after the second rotating ring 22 rotates, the second rotating ring can be elastically reset through the reset of the torsion spring 23, and a gap larger than the step boss 241 exists between the initial position of the clamping table 25 and the non-gradual change end of the gradual change ring 26, so that the step boss 241 can be clamped with the clamping table 25 when reset; since the gradual change ring 26 and the clamping table 25 are arranged in a staggered manner, the step boss 241 can be simultaneously contacted with the gradual change ring 26 and the clamping table 25, so that the step boss 241 is convenient to retract inwards and separate from the clamping table 25; the step boss 241 slides inside the step groove 243, as in the shape of fig. 10, to prevent the step boss 241 from completely coming out of the step groove 243;
because the first rotating ring 21 is fixedly installed on the main shaft 14, the main shaft 14 can drive the first rotating ring 21 to synchronously rotate while driving the mixing component to slowly rotate and mix, the first rotating ring 21 can simultaneously drive the base 24 to rotate with the stepped boss 241 when rotating, in the rotating process of the stepped boss 241, a part of the stepped boss 241 is contacted with the gradual changing ring 26, the stepped boss 241 gradually extrudes the spring 242 to slide towards the inside of the stepped groove 243 through the gradual changing shape of the gradual changing ring 26 until the stepped boss 241 moves to the other end of the gradual changing ring 26, the stepped boss 241 can spring out of the stepped groove 243 by means of the reset elasticity of the spring 242, then the other part of the stepped boss 241 is contacted with the clamping table 25, the stepped boss 241 pushes the clamping table 25 to rotate until a part of the stepped boss 241 is contacted with the gradual changing end of the gradual changing ring 26, so as to circulate until the other end of the stepped boss 241 is separated from the clamping table 25, the clamping table 25 can drive the second rotating ring 22 to rotate in the moving process, so as to drive the scraping plate 27 to rotate in the inside of the cooling groove 121, dirt is prevented from forming in the cooling groove 121, the inside, the crystallization efficiency of the solution is improved, and after the stepped boss 241 is separated from the clamping table 25, the clamping table 25 is separated from the clamping table 25 and the second rotating along with the reset spring 22, and the reset torsion spring 23 continuously rotates.
As shown in fig. 8, in the optimization of this embodiment, the number of the scrapers 27 is at least two, a plurality of scrapers 27 are arranged on the outer side of the second rotating ring 22, the left lower side scraper 27 is close to the inner wall of the cooling plate 12, no scrapers 27 are arranged on the right lower side inside the cooling groove 121, the included angle between two adjacent scrapers 27 is the same as the included angle between the rightmost scraper and the right lower corner inner wall of the cooling plate 12, and the shape of the scrapers 27 is an annular bar.
The number of the scrapers 27 is at least two, so that the rotating angle of the single scraper 27 is increased and reduced, the mechanical strain of parts such as the torsion spring 23 is reduced, the gradual travel of the gradual change end of the gradual change ring 26 is changed after the number of the scrapers 27 is increased, the gradual travel is matched with the rotating angle of the single scraper 27, the torsion spring 23 is beneficial to driving the second rotating ring 22 to reset after the rotating angle of the single scraper 27 is reduced, and the step boss 241 can be quickly abutted against the clamping table 25 when reset; the annular strip-shaped scraping plates 27 can reduce the resistance to the circulation of the cooling water, scrape the two sides of the cooling tank 121, mix dirt with the cooling water, and discharge the dirt along the connecting pipe 122, so that the dirt in the cooling water can be filtered and separated only by providing a filtering device at the outlet of the cooling water.
As shown in fig. 12, in the optimization of the present embodiment, the second rotating ring 22 is fixedly fitted inside with an L-shaped ring plate 231 that matches the torsion spring 23.
The space formed by the L-shaped ring plate 231 can internally deform the torsion spring 23 while protecting the torsion spring 23.
The above embodiments are merely illustrative of the principles of the present invention and its effectiveness, and are not intended to limit the invention. Modifications and variations may be made to the above-described embodiments by those skilled in the art without departing from the spirit and scope of the invention. Accordingly, it is intended that all equivalent modifications and variations of the invention be covered by the claims of this invention, which are within the skill of those skilled in the art, can be made without departing from the spirit and scope of the invention disclosed herein.
Claims (6)
1. The utility model provides a preparation facilities of electron level potassium hydroxide which characterized in that: the cooling device comprises a base, a cooling bin and a sealing cover, wherein the cooling bin is assembled at the upper end of the base, the sealing cover is hermetically arranged at the upper end of the cooling bin, a feed inlet and a discharge outlet are respectively formed in the front end and the rear end of the upper side of the cooling bin, a cooling mechanism is arranged on the inner side of the cooling bin and comprises a plurality of cooling plates, the cooling plates are uniformly assembled on the inner side of the cooling bin, cooling grooves are formed in the inner sides of the cooling plates, connecting pipes communicated with the cooling grooves are arranged on the left side and the right side of the upper part of the cooling plates, a plurality of cooling pipes are fixedly arranged on the two sides of the cooling bin, and the cooling pipes are detachably and fixedly connected with the connecting pipes;
the cooling bin is further provided with a mixing mechanism, the mixing mechanism comprises a driving motor, a main shaft and a plurality of mixing components, the driving motor is fixedly assembled at the upper end of the base, the main shaft is rotationally arranged at the inner side of the cooling bin, one end of the main shaft is in sealed rotation and penetrates through the cooling bin to be in transmission connection with the driving motor, the mixing components are uniformly assembled in the cooling bin, the mixing components are respectively positioned between two adjacent cooling plates, the mixing components are fixedly assembled at the main shaft, the cooling plates are matched with the inner side of the cooling bin in shape, and the lower side of each cooling plate is provided with a notch;
the cooling plate is characterized in that a scraping assembly is further arranged on the inner side of the cooling plate and comprises a first rotating ring, a second rotating ring, a torsion spring, a base, a stepped boss, a spring, a clamping table, a gradual change ring and a scraping plate, a rotating groove is formed in the middle of the cooling plate, the first rotating ring is rotationally and hermetically arranged in the rotating groove, a main shaft is fixedly connected with the inner side of the first rotating ring, the second rotating ring is rotationally and hermetically arranged in the cooling groove, the first rotating ring is positioned on the inner side of the second rotating ring, the torsion spring is assembled between the first rotating ring and the second rotating ring, one end of the torsion spring is fixedly connected with the inner wall of the cooling plate, the other end of the torsion spring is fixedly connected with the inner side of the second rotating ring, the base is fixedly arranged on the outer side of the first rotating ring, the base is provided with a stepped groove, one end of the stepped boss is slidingly arranged in the stepped groove, the spring is fixedly assembled between the stepped boss and the stepped groove, the clamping table is fixedly arranged on the inner side of the second rotating ring, the gradual change ring is assembled between the first rotating ring and the inner side of the cooling plate, the gradual change ring is gradually changed into a gradual change ring, the gradual change ring is fixedly connected with the inner side of the cooling plate, and the cooling plate is gradually changed into a gradual change ring, and is fixedly connected with the end of the cooling plate;
the number of the scrapers is at least two, a plurality of scrapers are arranged on the outer side of the second rotating ring, the scrapers are close to the inner wall of the cooling plate on the left lower side, the scrapers are not arranged on the right lower side inside the cooling tank, the included angle between two adjacent scrapers is the same as the included angle between the right-most scrapers and the inner wall of the right lower corner of the cooling plate, and the shape of each scraper is annular bar.
2. The apparatus for preparing electronic grade potassium hydroxide according to claim 1, wherein: the mixing assembly comprises two semicircular plates, wherein the two opposite ends of the semicircular plates are jointly provided with mounting rings matched with the main shaft, a plurality of partition plates are arranged on the front side and the rear side of each semicircular plate, the two partition plates are adjacent to each other, mounting holes are formed in the two partition plates, a plurality of mounting holes are respectively provided with bolts and nuts, the bottom of the cooling bin is semicircular, and the two semicircular plates are matched with the bottom of the cooling bin in shape.
3. The apparatus for preparing electronic grade potassium hydroxide according to claim 1, wherein: the inner side of the second rotating ring is fixedly provided with an L-shaped ring plate matched with the torsion spring.
4. The apparatus for preparing electronic grade potassium hydroxide according to claim 1, wherein: the connecting pipe outside rotates the cover and is equipped with the screw thread section of thick bamboo, the screw thread section of thick bamboo with cooling tube threaded connection, the screw thread section of thick bamboo with be equipped with the raw material area between the cooling tube, the connecting pipe outside with the screw thread section of thick bamboo inboard all is equipped with mutually supporting sealing ring.
5. The apparatus for preparing electronic grade potassium hydroxide according to claim 1, wherein: and a plurality of treatment areas are respectively arranged on the front side and the rear side of the cooling plate, and a plurality of treatment areas are subjected to grinding thinning treatment.
6. A preparation method of electronic grade potassium hydroxide is characterized in that: the method comprises the following steps:
s1, introducing a 25% -30% low-concentration solution product prepared from industrial-grade potassium hydroxide into evaporation equipment, and evaporating and concentrating a 25% -30% potassium hydroxide solution to a 50% -55% potassium hydroxide saturated solution through evaporation and concentration;
s2, introducing 7-12 ℃ cooling water into a crystallizer, and then introducing 50-55% potassium hydroxide saturated solution into the crystallizer for cooling treatment to reduce the solubility of potassium hydroxide in the potassium hydroxide saturated solution, wherein the crystallizer is composed of the electronic-grade potassium hydroxide preparation device according to any one of claims 1-5;
s3, cooling the mixed solution by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and then introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
s4, adding pure water into the potassium hydroxide crystals separated by the disc type centrifugal machine to dissolve the potassium hydroxide crystals, and obtaining the electronic-grade potassium hydroxide solution.
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Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN204767559U (en) * | 2015-05-28 | 2015-11-18 | 宁波大学 | Energy -conserving cooling crystallizer |
| CN204767554U (en) * | 2015-05-27 | 2015-11-18 | 江苏汉光生物工程有限公司 | Crystallizer |
| FR3030306A1 (en) * | 2014-12-17 | 2016-06-24 | Fives Cail Babcock | MIXING DEVICE AND THERMAL EXCHANGE |
| CN206081726U (en) * | 2016-10-17 | 2017-04-12 | 江西氟塑防腐设备集团有限公司 | Novel high -efficient anticorrosive board -like continuous crystallizer of scraping |
| CN211854951U (en) * | 2019-10-25 | 2020-11-03 | 湖北银昌科技有限公司 | High viscosity medium cooling device |
| CN212327460U (en) * | 2020-05-18 | 2021-01-12 | 四川能投建工集团设计研究院有限公司 | A reaction crystallizer tank for producing potassium nitrate |
| CN113860336A (en) * | 2021-10-28 | 2021-12-31 | 华融化学股份有限公司 | Preparation method of electronic-grade potassium hydroxide |
-
2022
- 2022-09-14 CN CN202211113167.XA patent/CN115304081B/en active Active
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| FR3030306A1 (en) * | 2014-12-17 | 2016-06-24 | Fives Cail Babcock | MIXING DEVICE AND THERMAL EXCHANGE |
| CN204767554U (en) * | 2015-05-27 | 2015-11-18 | 江苏汉光生物工程有限公司 | Crystallizer |
| CN204767559U (en) * | 2015-05-28 | 2015-11-18 | 宁波大学 | Energy -conserving cooling crystallizer |
| CN206081726U (en) * | 2016-10-17 | 2017-04-12 | 江西氟塑防腐设备集团有限公司 | Novel high -efficient anticorrosive board -like continuous crystallizer of scraping |
| CN211854951U (en) * | 2019-10-25 | 2020-11-03 | 湖北银昌科技有限公司 | High viscosity medium cooling device |
| CN212327460U (en) * | 2020-05-18 | 2021-01-12 | 四川能投建工集团设计研究院有限公司 | A reaction crystallizer tank for producing potassium nitrate |
| CN113860336A (en) * | 2021-10-28 | 2021-12-31 | 华融化学股份有限公司 | Preparation method of electronic-grade potassium hydroxide |
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| CN115304081A (en) | 2022-11-08 |
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