CN115304081A - 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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- CN115304081A CN115304081A CN202211113167.XA CN202211113167A CN115304081A CN 115304081 A CN115304081 A CN 115304081A CN 202211113167 A CN202211113167 A CN 202211113167A CN 115304081 A CN115304081 A CN 115304081A
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- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 title claims abstract description 236
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- 238000001816 cooling Methods 0.000 claims abstract description 182
- 239000013078 crystal Substances 0.000 claims abstract description 20
- 239000000498 cooling water Substances 0.000 claims abstract description 16
- 238000001704 evaporation Methods 0.000 claims abstract description 12
- 239000012047 saturated solution Substances 0.000 claims abstract description 12
- 238000000034 method Methods 0.000 claims abstract description 10
- 230000008020 evaporation Effects 0.000 claims abstract description 8
- 239000011259 mixed solution Substances 0.000 claims abstract description 8
- 239000000243 solution Substances 0.000 claims abstract description 8
- 238000011282 treatment Methods 0.000 claims abstract description 8
- 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
- 230000008859 change Effects 0.000 claims description 48
- 238000002156 mixing Methods 0.000 claims description 31
- 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
- 230000007246 mechanism Effects 0.000 claims description 8
- 238000007789 sealing Methods 0.000 claims description 8
- 238000012545 processing Methods 0.000 claims description 6
- 230000005540 biological transmission Effects 0.000 claims description 4
- 238000000227 grinding Methods 0.000 claims description 3
- 125000004122 cyclic group Chemical group 0.000 claims description 2
- 238000002425 crystallisation Methods 0.000 abstract description 7
- 230000008025 crystallization Effects 0.000 abstract description 7
- 230000000694 effects Effects 0.000 abstract description 2
- 238000009434 installation Methods 0.000 description 6
- 238000005192 partition Methods 0.000 description 6
- 238000007790 scraping Methods 0.000 description 6
- 238000005457 optimization Methods 0.000 description 5
- 238000012546 transfer Methods 0.000 description 5
- 238000003756 stirring Methods 0.000 description 4
- 230000008569 process Effects 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002349 favourable effect Effects 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
- 238000005342 ion exchange Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 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
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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, which comprises 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 a 50-55% potassium hydroxide saturated solution through evaporation and concentration; introducing cooling water with the temperature of 7-12 ℃ into a crystallizer, and then introducing a potassium hydroxide saturated solution with the concentration of 50% -55% into the crystallizer for cooling treatment to reduce the solubility of potassium hydroxide in the potassium hydroxide saturated solution; cooling the solution by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disk centrifuge for crystal separation; adding pure water into potassium hydroxide crystals separated by a disc centrifuge for dissolving to obtain an 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 method and a device for preparing electronic-grade potassium hydroxide.
Background
With the domestic market demand and the development of the semiconductor and electronic industry, the quality requirement of customers on the potassium hydroxide solution is higher and higher, industrial-grade potassium hydroxide cannot meet the requirement, and the industrial-grade potassium hydroxide needs to be purified to improve the quality; at present, the electronic-grade potassium hydroxide is generally produced by firstly preparing potassium hydroxide into a potassium hydroxide solution, then removing heavy metals and sodium ions by adopting methods such as ion exchange or cooling freezing crystallization, and the like.
Disclosure of Invention
The purpose of the invention is: aims to provide a method and a device for preparing electronic-grade potassium hydroxide, which are used for solving the problems in the background technology.
In order to achieve the technical purpose, the technical scheme adopted by the invention is as follows:
a preparation method of 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 cooling water of 7-12 ℃ into a crystallizer, and then introducing a potassium hydroxide saturated solution of 50% -55% concentration into the crystallizer for cooling treatment to reduce the solubility of potassium hydroxide in the potassium hydroxide saturated solution;
s3, cooling by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
and S4, adding pure water to dissolve the potassium hydroxide crystals separated by the disk-type centrifuge to obtain the electronic-grade potassium hydroxide solution.
The utility model provides a preparation facilities of electron level potassium hydroxide, is applied to step S2 of a preparation method of electron level potassium hydroxide, includes base, cooling bin and closing cap, the cooling bin assemble in the base upper end, the closing cap is sealed to be located the cooling bin upper end, feed inlet and discharge gate have been seted up respectively at both ends around the cooling bin upside, cooling bin inboard is equipped with cooling body, cooling body includes a plurality of cooling plates, and is a plurality of the cooling plate evenly assemble in the cooling bin is inboard, and is a plurality of the cooling bath has all been seted up to the cooling plate inboard, the cooling plate upper portion left and right sides all be equipped with the connecting pipe that the cooling bath communicates, the fixed a plurality of cooling tubes that are equipped with in cooling bin both sides, the cooling tube with fixed connection can be dismantled to the connecting pipe.
Preferably, the cooling bin still is equipped with mixing mechanism, mixing mechanism includes driving motor, main shaft and a plurality of mixing subassembly, driving motor fixed assembly in the base upper end, the main shaft rotates to be located the cooling bin is inboard, the sealed rotation of main shaft one end runs through the cooling bin with the driving motor transmission is connected, and is a plurality of mixing subassembly evenly assemble in inside the cooling bin, it is a plurality of mixing subassembly is located two respectively adjacently between the cooling plate, a plurality of mixing subassembly all fixed assembly in the main shaft, the cooling plate with the inboard shape phase-match in cooling bin, the notch has been seted up to the cooling plate downside.
Preferably, the mixing subassembly includes two semicircle boards, two the relative one end of semicircle board be equipped with jointly with main shaft assorted collar, two both sides all are equipped with a plurality of baffles, two around the semicircle board adjacent two on the semicircle board the mounting hole has all been seted up to the baffle, and is a plurality of the mounting hole all is equipped with bolt and nut, cooling storehouse bottom is semi-circular, two the semicircle board all with cooling storehouse bottom shape matches.
Preferably, the cooling plate inboard still is equipped with strikes off the subassembly, strike off the subassembly and include first change ring, second change ring, torsional spring, base station, ladder boss, spring, ka tai, gradual change ring sum scraper blade, the rotary trough has been seted up at the cooling plate middle part, first change ring rotary seal locates the rotary trough, the main shaft with the inboard fixed connection of first change ring, second change ring rotary seal locates inside the cooling trough, first change ring is located the second change ring is inboard, the torsional spring assemble in first change ring with between the second change ring, torsional spring one end with cooling plate inner wall fixed connection, the torsional spring other end with the inboard fixed connection of second change ring, the base station is fixed locate the first change ring outside, the ladder groove has been seted up to the base station, ladder boss one end slides and locates the ladder inslot portion, the spring is fixed assemble in the ladder boss with between the ladder groove, ka tai fixed locate the second change ring is inboard, the assembly in between the first change ring with the second change ring with between the second change ring, gradually the fixed joint gradually the inner wall is not gathered together with the tip with the second change ring.
Preferably, scraper blade quantity is two at least, and is a plurality of the scraper blade is located the second swivel becket outside, left downside the scraper blade with the cooling plate inner wall is close to, the inside right downside of cooling bath does not set up the scraper blade, two adjacent contained angle between the scraper blade and rightmost side scraper blade with the contained angle is the same between the cooling plate lower right corner inner wall, the scraper blade shape is cyclic annular bar.
Preferably, an L-shaped ring plate matched with the torsion spring is fixedly assembled on the inner side of the second rotating ring.
Preferably, the connecting pipe outside is rotated the cover and is equipped with a screw thread section of thick bamboo, a screw thread section of thick bamboo with cooling tube threaded connection, a screw thread section of thick bamboo with be equipped with the thread seal area between the cooling tube, the connecting pipe outside with a screw thread section of thick bamboo inboard all is equipped with the sealing ring that matches each other.
Preferably, a plurality of processing areas are arranged on the front side and the rear side of the cooling plate, and the processing areas are ground and thinned.
The invention has the advantages that: 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 mode, the plurality of rotating semicircular plates can uniformly stir the passing potassium hydroxide solution, the surfaces of the cooling plates can be scraped, precipitated crystals are prevented from being attached to the cooling plates, the cooling efficiency is improved, and the semicircular plates are attached to the cooling plates, so that the potassium hydroxide solution can be driven to be transported around the inside of the cooling bin, the moving path of the potassium hydroxide solution is increased, the heat exchange time between 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 cycle and rotate, strike off the inside dirt of cooling plate, the scraper blade of reciprocating scraping can also make dirt and cooling water mix, makes inside its discharge cooling plate, avoids the cooling water scale deposit, makes heat exchange efficiency improve.
Drawings
The invention is further illustrated by the non-limiting examples given in the figures.
FIG. 1 is a schematic structural diagram of a first embodiment of an apparatus for preparing electronic-grade potassium hydroxide according to the present invention;
FIG. 2 is a schematic view of 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 of a partial cross-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 at A in FIG. 3;
FIG. 5 is a schematic view of a partial cross-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 of FIG. 5;
FIG. 7 is a schematic structural view of a cooling plate in a third embodiment of the apparatus for preparing electronic-grade potassium hydroxide according to the present invention;
FIG. 8 is a schematic cross-sectional view of a cooling plate in a third embodiment of an apparatus for preparing electronic-grade potassium hydroxide according to the present invention;
FIG. 9 is a schematic cross-sectional view of a cooling plate in a third embodiment of an apparatus for preparing electronic-grade potassium hydroxide according to the present invention;
FIG. 10 is an enlarged schematic view at C of FIG. 9;
FIG. 11 is a third schematic sectional view of a cooling plate in a third embodiment of the apparatus for preparing electronic-grade potassium hydroxide according to the present invention;
FIG. 12 is an enlarged schematic view at D of FIG. 11;
the main element symbols are as follows:
the device comprises a base 1, a cooling bin 11, a cover 111, a feed inlet 112, a discharge outlet 113, a cooling plate 12, a cooling groove 121, a connecting pipe 122, a cooling pipe 123, a notch 124, a threaded cylinder 125, a sealing ring 126, a treatment area 127, a driving motor 13, a main shaft 14, a semicircular plate 15, a mounting ring 151, a partition plate 152, a first rotating ring 21, a rotating groove 211, a second rotating ring 22, a torsion spring 23, an L-shaped ring plate 231, a base 24, a stepped boss 241, a spring 242, a stepped groove 243, a clamping table 25, a gradual change ring 26 and a scraper 27.
Detailed Description
In order that those skilled in the art can better understand the present invention, the following technical solutions are 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 cooling water with the temperature of 7-12 ℃ into a crystallizer, and then introducing a 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;
s3, cooling by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
and S4, adding pure water to dissolve the potassium hydroxide crystals separated by the disk-type centrifuge to obtain the electronic-grade potassium hydroxide solution.
The first embodiment is as follows:
as shown in fig. 1-4, the apparatus for preparing electronic-grade potassium hydroxide of the present invention is applied to step S2 of a method for preparing electronic-grade potassium hydroxide, and includes a base 1, a cooling chamber 11, and a sealing cover 111, wherein the cooling chamber 11 is assembled on the upper end of the base 1, the sealing cover 111 is hermetically disposed on the upper end of the cooling chamber 11, a feed inlet 112 and a discharge outlet 113 are respectively disposed at front and rear ends of the upper side of the cooling chamber 11, a cooling mechanism is disposed inside the cooling chamber 11, the cooling mechanism includes a plurality of cooling plates 12, the plurality of cooling plates 12 are uniformly assembled inside the cooling chamber 11, cooling grooves 121 are disposed inside the plurality of cooling plates 12, connecting pipes 122 communicated with the cooling grooves 121 are disposed on left and right sides of the upper portion of the cooling plates 12, a plurality of cooling pipes 123 are fixedly disposed on two sides of the cooling chamber 11, and the cooling pipes 123 are detachably connected to the connecting pipes 122.
The blending components and the cooling plates 12 in the cooling bin 11 are distributed in a staggered manner, and the blending components are arranged at the positions close to the feeding hole 112 and the discharging hole 112 and can be used for stirring the entering and exiting solution; the cooling pipes 123 on the left and right sides are used for externally connecting a cooling water output device and a recovery device, and are conventional technical means; this device is when carrying out the crystallization to potassium hydroxide solution, earlier let in potassium hydroxide solution from the feed inlet 112 department of cooling bin 11, continuously let in the cooling water through a plurality of cooling tubes 123 to the cooling bath 121 inside of a plurality of cooling plates 12 simultaneously, the cooling water can be followed cooling plate 12 one side connecting pipe 122 and got into, then flow out from the connecting pipe 122 of cooling plate 12 opposite side, potassium hydroxide solution gets into cooling bin 11 inside back, notch 124 that can pass a plurality of cooling plates 12 in proper order flows to discharge gate 113 direction, a plurality of mixing subassemblies of in-process pass through driving motor 13 transmission drive and rotate, the mixing subassembly slowly rotates and carries out the mixing stirring to the potassium hydroxide solution in the heat transfer, make the even heat transfer of potassium hydroxide solution, and the heat exchange efficiency is improved, and the efficiency of crystallization is increased.
As shown in fig. 4, in the present embodiment, a threaded cylinder 125 is rotatably sleeved outside the connecting pipe 122, the threaded cylinder 125 is in threaded connection with the cooling pipe 123, a raw material tape is assembled between the threaded cylinder 125 and the cooling pipe 123, and mutually matching sealing rings 126 are disposed outside the connecting pipe 122 and inside the threaded cylinder 125.
The thread seal area can increase the leakproofness of threaded connection department, lasts the screw thread through two sides screw thread section of thick bamboo 125 and rotates the cover and locate cooling tube 123, can make two sealing ring 126 subassemblies be close to this seals the processing through two sealing ring 126 to connecting, and 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 the present embodiment, a plurality of processing areas 127 are disposed on both the front and rear sides of the cooling plate 12, and the plurality of processing areas 127 are subjected to grinding and thinning processes.
The outer side 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 is facilitated, and the crystallization efficiency of the potassium hydroxide solution is improved.
Example two:
as shown in fig. 5-6, for the further optimization of the first embodiment, the blending component includes two semicircular plates 15, two opposite ends of the semicircular plates 15 are provided with a mounting ring 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 chamber 11 is semicircular, and the two semicircular plates 15 are matched with the bottom of the cooling chamber 11 in shape.
The two semicircular plates 15 can be fixedly installed together through the plurality of installation holes by means of bolts and nuts, and at the moment, the two installation rings 151 can be fixedly clamped on the main shaft 14, so that the driving motor 13 can be started to drive the plurality of blending 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 each semicircular plate 15 are respectively provided with the plurality of partition plates 152, the semicircular plates 15 are isolated by the plurality of partition plates 152 to form a plurality of fan-shaped areas, after the potassium hydroxide solution is introduced into the cooling bin 11, the potassium hydroxide solution cannot slightly cross the uniform mixing assembly from the lower side, the areas isolated by the plurality of partition plates 152 rotate, when the semicircular plates 15 rotate to the upper side, the potassium hydroxide solution on the upper side can enter the other side of each semicircular plate 15 from the side edge, then continuously rotate along the semicircular plates 15, and when the semicircular plates rotate to the lower side, the potassium hydroxide solution passes through the notches 124 of the cooling plates 12 and flows into one side of the next semicircular plate 15 to be sequentially circulated, so that the flow path of the potassium hydroxide solution can be increased, the potassium hydroxide solution is fully contacted with the cooling plates 12 for heat exchange, and the heat exchange effect is improved;
when a plurality of cooling plates 12 carry out the heat transfer, the phenomenon that the crystal appeared can appear in the position that is close to cooling plates 12, the cooling plates can be pressed close to the crystal that leads to appearing, can reduce the efficiency of potassium hydroxide solution and the heat transfer of cooling plates 12 like this, only need press close to cooling plates 12 installation with semicircle board 15 when installation semicircle board 15 for this reason, when the mixing subassembly carries out the slow stirring mixing, can scrape the clearance to the surface of cooling plates 12 like this, prevent that the crystal that appears from pressing close to cooling plates 12 side, improve cooling heat transfer's efficiency.
Example three:
as shown in fig. 7-12, for further optimization of the first embodiment, or simultaneously with optimization and improvement of the second embodiment, more beneficial effects can be achieved, a scraping assembly is further disposed inside 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 step boss 241, a spring 242, a clamping platform 25, a gradual change ring 26, and a scraper 27, a rotating groove 211 is disposed in the middle of the cooling plate 12, the first rotating ring 21 is rotatably and hermetically disposed in the rotating groove 211, the main shaft 14 is fixedly connected to the inside of the first rotating ring 21, the second rotating ring is rotatably and hermetically disposed inside the cooling groove 121, the first rotating ring 21 is disposed inside 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 a 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, a stepped groove 243 is formed in the base 24, one end of a stepped boss 241 is slidably arranged in the stepped groove 243, the spring 242 is fixedly assembled between the stepped boss 241 and the stepped groove 243, the clamping table 25 is fixedly arranged on the inner side of the second rotating ring 22, the 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 unclosed ring, the inner side of one end of the gradual change ring 26 gradually gathers to the end, the gradual change ring 26 and the clamping table 25 are arranged in a staggered mode, the stepped boss 241 is matched with the gradual change ring 26 and the clamping table 25, and the scraper 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 form scale, and the scale 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 independent descaling treatment of the cooling plate 12 is quite troublesome, so that the cooling plate 12 is optimized and improved;
by the dynamic seal installation of the first rotating ring 21 and the second rotating ring 22, 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 tank 121, so that the second rotating ring 22 can be reset through the resetting elasticity of the torsion spring 23 after rotating, and the interval larger than the size of the stepped boss 241 exists between the initial position of the clamping platform 25 and the non-gradual change end of the gradual change ring 26, so that the stepped boss 241 can be clamped with the clamping platform 25 when resetting; because the gradual change ring 26 and the clamping platform 25 are arranged in a staggered manner, the stepped boss 241 can be simultaneously contacted with the gradual change ring 26 and the clamping platform 25, so that the stepped boss 241 is conveniently retracted and separated from the clamping platform 25; the step boss 241 slides inside the step groove 243, and as in the shape shown in fig. 10, the step boss 241 can be prevented from completely escaping from the step groove 243;
the first rotating ring 21 is fixedly installed on the main shaft 14, so the main shaft 14 can drive the first rotating ring 21 to synchronously rotate while driving the blending component to slowly rotate and blend, the first rotating ring 21 can simultaneously drive the base station 24 and the stepped boss 241 to rotate when rotating, during the rotation process of the stepped boss 241, a part of the stepped boss 241 is in contact with the gradual change ring 26, the stepped boss 241 gradually extrudes the spring 242 to slide towards the inside of the stepped groove 243 through the gradual change shape of the gradual change ring 26 until the stepped boss 241 moves to the other end of the gradual change ring 26, the stepped boss 241 is popped out of the stepped groove 243 by the resetting elasticity of the spring 242, then the other part of the stepped boss 241 is in contact with the clamping platform 25, the stepped boss 241 pushes the clamping platform 25 to rotate and move until a part of the stepped boss 241 is in contact with one end of the gradual change ring 26, so as to circulate until the other end of the stepped boss 241 is separated from the clamping platform 25, the clamping platform 25 drives the second rotating ring 22 to rotate during the movement process, so as to drive the scraping plate 27 to rotate and scrape the wall in the cooling groove 121, thereby preventing the formation of the cooling groove 121, improving the efficiency of potassium hydroxide, and the potassium hydroxide solution, and the rotating platform 23 can continuously return to the cooling solution by the torsion spring 27, and the rotating platform 23 can continuously return the clamping platform to the clamping platform.
As shown in fig. 8, in the optimization of this embodiment, the number of the scrapers 27 is at least two, the plurality of scrapers 27 are disposed outside the second rotating ring 22, the left lower scraper 27 is close to the inner wall of the cooling plate 12, the scraper 27 is not disposed at the lower right side inside the cooling groove 121, an included angle between two adjacent scrapers 27 is the same as an included angle between the rightmost scraper and the inner wall of the lower right corner of the cooling plate 12, and the scraper 27 is in the shape of an annular strip.
The number of the scrapers 27 is at least two, so that the rotating angle of a single scraper 27 during scraping is increased and reduced, the mechanical strain of parts such as the torsion spring 23 is reduced, after the number of the scrapers 27 is increased, the gradual change stroke of the gradual change end of the gradual change ring 26 is changed, the gradual change stroke is matched with the rotating angle of the single scraper 27, after the rotating angle of the single scraper 27 is reduced, the torsion spring 23 is favorable for driving the second rotating ring 22 to reset, and the stepped boss 241 can be quickly abutted to the clamping table 25 when being reset; and the annular strip-shaped scraper 27 can reduce the resistance to the circulation of the cooling water, and when scraping both sides in the cooling tank 121, the dirt and the cooling water are mixed to be discharged along the connecting pipe 122, and the dirt in the cooling water can be filtered and separated only by arranging a filtering device at the outlet of the cooling water.
As shown in fig. 12, in the present embodiment, an L-shaped ring plate 231 matched with the torsion spring 23 is fixedly assembled inside the second rotating ring 22.
The space formed by the L-shaped ring plate 231 enables the torsion spring 23 to be deformed therein while protecting the torsion spring 23.
The foregoing embodiments are merely illustrative of the principles of the present invention and its efficacy, and are not to be construed as limiting the invention. Any person skilled in the art can modify or change the above-mentioned embodiments without departing from the spirit and scope of the present invention. Accordingly, it is intended that all equivalent modifications or changes which may be made by those skilled in the art without departing from the spirit and scope of the present invention as defined in the appended claims.
Claims (9)
1. A preparation method of electronic-grade potassium hydroxide is characterized by comprising the following steps: 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 cooling water with the temperature of 7-12 ℃ into a crystallizer, and then introducing a 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;
s3, cooling by a crystallizer to obtain a potassium hydroxide mixed solution containing potassium hydroxide crystals, and introducing the potassium hydroxide mixed solution containing potassium hydroxide crystals into a disc centrifuge for crystal separation;
and S4, adding pure water to dissolve the potassium hydroxide crystals separated by the disk-type centrifuge to obtain the electronic-grade potassium hydroxide solution.
2. A preparation device of electronic-grade potassium hydroxide is applied to a step S2 of a preparation method of the electronic-grade potassium hydroxide, and is characterized in that: including base, cooling bin and closing cap, the assembly of cooling bin in the base upper end, the closing cap is sealed to be located the cooling bin upper end, feed inlet and discharge gate have been seted up respectively at both ends around the cooling bin upside, the cooling bin inboard is equipped with cooling body, cooling body includes a plurality of cooling plates, and is a plurality of the cooling plate evenly assemble in the cooling bin is inboard, and is a plurality of the cooling bath has all been seted up to the cooling plate inboard, the cooling plate upper portion left and right sides all be equipped with the connecting pipe that the cooling bath communicates mutually, the fixed a plurality of cooling tubes that are equipped with in cooling bin both sides, the cooling tube with fixed connection can be dismantled to the connecting pipe.
3. The apparatus of claim 2, wherein: the cooling bin still is equipped with mixing mechanism, mixing mechanism includes driving motor, main shaft and a plurality of mixing subassembly, driving motor fixed assembly in the base upper end, the main shaft rotates to be located the cooling bin is inboard, the sealed rotation of main shaft one end runs through the cooling bin with the driving motor transmission is connected, and is a plurality of mixing subassembly evenly assemble in inside the cooling bin, it is a plurality of mixing subassembly is located two adjacent respectively between the cooling plate, it is a plurality of mixing subassembly all fixed assembly in the main shaft, the cooling plate with the inboard shape phase-match in cooling bin, the notch has been seted up to the cooling plate downside.
4. The apparatus of claim 3, wherein: mixing subassembly includes two semicircle boards, two the relative one end of semicircle board be equipped with jointly with main shaft assorted collar, two both sides all are equipped with a plurality of baffles around the semicircle board, two adjacent two on the semicircle board the mounting hole has all been seted up to the baffle, and is a plurality of the mounting hole all is equipped with bolt and nut, the cooling storehouse bottom is semi-circular, two the semicircle board all with the form of cooling storehouse bottom matches.
5. The apparatus of claim 3, wherein: the utility model discloses a cooling plate, including cooling plate, torsional spring, base station, ladder boss, spring, ka tai, gradual change ring and scraper blade, the cooling plate inboard still is equipped with strikes off the subassembly, strike off the subassembly and include first rotating ring, second rotating ring, torsional spring, base station, ladder boss, spring, ka tai, gradual change ring and scraper blade, the rotating groove has been seted up at the cooling plate middle part, first rotating ring rotary seal locates the rotating groove, the second rotating ring rotary seal locates inside the cooling groove, first rotating ring is located the second rotating ring is inboard, the torsional spring assemble in first rotating ring with between the second rotating ring, torsional spring one end with cooling plate inner wall fixed connection, the torsional spring other end with the inboard fixed connection of second rotating ring, the base station is fixed locate the first rotating ring outside, the ladder groove has been seted up to the base station, ladder boss one end is slided and is located in the ladder inslot, the spring fixed assembly in the ladder boss with between the ladder groove, ka tai fixed locate the second rotating ring is inboard, the scraper blade assembly in the first rotating ring with between the second rotating ring with between the base station, the gradual change ring with the cooling plate inner wall fixed connection gradually connect gradually, gradually the gradual change ring is gradually the inboard, gradually the gradual change ring is not set up with the gradual change the second rotating ring, gradually the end is all set up with the gradual change the inboard with the gradual change platform, gradually the second rotating ring, gradually the inboard with the end is the gradual change is the inboard.
6. The apparatus of claim 5, wherein: scraper blade quantity is two at least, and is a plurality of the scraper blade is located the second rotating ring outside, left downside the scraper blade with the cooling plate inner wall is close to, the inside right downside of cooling bath does not set up the scraper blade, two adjacent contained angle and rightmost side scraper blade between the scraper blade with the contained angle is the same between the cooling plate lower right corner inner wall, the scraper blade shape is cyclic annular bar.
7. The apparatus of claim 5, wherein: and an L-shaped annular plate matched with the torsion spring is fixedly assembled on the inner side of the second rotating ring.
8. The apparatus of claim 2, wherein: the connecting pipe outside is rotated the cover and is equipped with a screw thread section of thick bamboo, a screw thread section of thick bamboo with cooling tube threaded connection, a screw thread section of thick bamboo with be equipped with the thread seal area between the cooling tube, the connecting pipe outside with screw thread section of thick bamboo inboard all is equipped with the sealing ring that matches each other.
9. The apparatus of claim 2, wherein: and a plurality of processing areas are arranged on the front side and the rear side of the cooling plate, and are subjected to grinding and thinning treatment.
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| CN202211113167.XA CN115304081B (en) | 2022-09-14 | 2022-09-14 | Preparation method and device of electronic-grade potassium hydroxide |
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| CN202211113167.XA CN115304081B (en) | 2022-09-14 | 2022-09-14 | Preparation method and device of electronic-grade potassium hydroxide |
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| CN211854951U (en) * | 2019-10-25 | 2020-11-03 | 湖北银昌科技有限公司 | High viscosity medium cooling device |
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| 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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| 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 |
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| CN115304081B (en) | 2024-03-01 |
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