CN117886335A - Process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as raw material - Google Patents
Process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as raw material Download PDFInfo
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- CN117886335A CN117886335A CN202410288246.7A CN202410288246A CN117886335A CN 117886335 A CN117886335 A CN 117886335A CN 202410288246 A CN202410288246 A CN 202410288246A CN 117886335 A CN117886335 A CN 117886335A
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- potassium
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- NROKBHXJSPEDAR-UHFFFAOYSA-M potassium fluoride Chemical compound [F-].[K+] NROKBHXJSPEDAR-UHFFFAOYSA-M 0.000 title claims abstract description 76
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 title claims abstract description 60
- 239000011698 potassium fluoride Substances 0.000 title claims abstract description 38
- 235000003270 potassium fluoride Nutrition 0.000 title claims abstract description 38
- 239000006229 carbon black Substances 0.000 title claims abstract description 30
- 239000002253 acid Substances 0.000 title claims abstract description 25
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 25
- 239000002994 raw material Substances 0.000 title claims abstract description 20
- 238000003756 stirring Methods 0.000 claims abstract description 88
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims abstract description 44
- 239000012065 filter cake Substances 0.000 claims abstract description 30
- 238000001914 filtration Methods 0.000 claims abstract description 30
- 238000010438 heat treatment Methods 0.000 claims abstract description 24
- 239000001103 potassium chloride Substances 0.000 claims abstract description 22
- 235000011164 potassium chloride Nutrition 0.000 claims abstract description 22
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims abstract description 21
- 239000011591 potassium Substances 0.000 claims abstract description 21
- 229910052700 potassium Inorganic materials 0.000 claims abstract description 21
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 13
- 239000002002 slurry Substances 0.000 claims abstract description 12
- 238000005406 washing Methods 0.000 claims abstract description 11
- 239000000047 product Substances 0.000 claims abstract description 10
- 239000000706 filtrate Substances 0.000 claims abstract description 9
- KWYUFKZDYYNOTN-UHFFFAOYSA-M Potassium hydroxide Chemical compound [OH-].[K+] KWYUFKZDYYNOTN-UHFFFAOYSA-M 0.000 claims abstract description 6
- 239000011268 mixed slurry Substances 0.000 claims abstract description 5
- 238000005192 partition Methods 0.000 claims description 63
- 239000007788 liquid Substances 0.000 claims description 39
- 239000002699 waste material Substances 0.000 claims description 33
- 238000003825 pressing Methods 0.000 claims description 13
- 238000001035 drying Methods 0.000 claims description 9
- 238000001514 detection method Methods 0.000 claims description 7
- 238000007599 discharging Methods 0.000 claims description 7
- 238000000034 method Methods 0.000 claims description 7
- 230000001360 synchronised effect Effects 0.000 claims description 7
- 238000005485 electric heating Methods 0.000 claims description 5
- 238000009423 ventilation Methods 0.000 claims description 5
- 235000012239 silicon dioxide Nutrition 0.000 claims description 4
- 230000000712 assembly Effects 0.000 claims description 3
- 238000000429 assembly Methods 0.000 claims description 3
- 230000001105 regulatory effect Effects 0.000 description 13
- 230000001276 controlling effect Effects 0.000 description 3
- 230000013011 mating Effects 0.000 description 3
- 239000000843 powder Substances 0.000 description 3
- 235000017166 Bambusa arundinacea Nutrition 0.000 description 2
- 235000017491 Bambusa tulda Nutrition 0.000 description 2
- 241001330002 Bambuseae Species 0.000 description 2
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 235000015334 Phyllostachys viridis Nutrition 0.000 description 2
- 239000004115 Sodium Silicate Substances 0.000 description 2
- 239000011425 bamboo Substances 0.000 description 2
- 239000011521 glass Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- NTHWMYGWWRZVTN-UHFFFAOYSA-N sodium silicate Chemical compound [Na+].[Na+].[O-][Si]([O-])=O NTHWMYGWWRZVTN-UHFFFAOYSA-N 0.000 description 2
- 229910052911 sodium silicate Inorganic materials 0.000 description 2
- ASZZHBXPMOVHCU-UHFFFAOYSA-N 3,9-diazaspiro[5.5]undecane-2,4-dione Chemical compound C1C(=O)NC(=O)CC11CCNCC1 ASZZHBXPMOVHCU-UHFFFAOYSA-N 0.000 description 1
- VXEGSRKPIUDPQT-UHFFFAOYSA-N 4-[4-(4-methoxyphenyl)piperazin-1-yl]aniline Chemical compound C1=CC(OC)=CC=C1N1CCN(C=2C=CC(N)=CC=2)CC1 VXEGSRKPIUDPQT-UHFFFAOYSA-N 0.000 description 1
- BPQQTUXANYXVAA-UHFFFAOYSA-N Orthosilicate Chemical compound [O-][Si]([O-])([O-])[O-] BPQQTUXANYXVAA-UHFFFAOYSA-N 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 1
- YKTSYUJCYHOUJP-UHFFFAOYSA-N [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] Chemical compound [O--].[Al+3].[Al+3].[O-][Si]([O-])([O-])[O-] YKTSYUJCYHOUJP-UHFFFAOYSA-N 0.000 description 1
- 230000002745 absorbent Effects 0.000 description 1
- 239000002250 absorbent Substances 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 230000001174 ascending effect Effects 0.000 description 1
- 238000010009 beating Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000378 calcium silicate Substances 0.000 description 1
- 229910052918 calcium silicate Inorganic materials 0.000 description 1
- OYACROKNLOSFPA-UHFFFAOYSA-N calcium;dioxido(oxo)silane Chemical compound [Ca+2].[O-][Si]([O-])=O OYACROKNLOSFPA-UHFFFAOYSA-N 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 238000005536 corrosion prevention Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000009713 electroplating Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000004907 flux Effects 0.000 description 1
- 235000013305 food Nutrition 0.000 description 1
- 229910021485 fumed silica Inorganic materials 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- 239000000575 pesticide Substances 0.000 description 1
- 229910052573 porcelain Inorganic materials 0.000 description 1
- 235000019643 salty taste Nutrition 0.000 description 1
- 229910002027 silica gel Inorganic materials 0.000 description 1
- 239000000741 silica gel Substances 0.000 description 1
- RMAQACBXLXPBSY-UHFFFAOYSA-N silicic acid Chemical compound O[Si](O)(O)O RMAQACBXLXPBSY-UHFFFAOYSA-N 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 239000005049 silicon tetrachloride Substances 0.000 description 1
- 238000005476 soldering Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Landscapes
- Silicon Compounds (AREA)
Abstract
The invention discloses a process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material, which comprises the following steps: dissolving and filtering potassium chloride to obtain a potassium chloride solution, and step two: injecting potassium chloride solution into a reaction barrel to react with fluosilicic acid solution, filtering and washing after the reaction to obtain a potassium fluosilicate filter cake, and step three: adding water into the potassium fluosilicate filter cake, stirring to obtain potassium fluosilicate slurry, heating the potassium fluosilicate slurry, and then injecting potassium hydroxide solution for reaction; step four: after the reaction is finished, the obtained mixed slurry is filtered to obtain a silica filter cake and a filtrate containing potassium fluoride, the silica filter cake is washed and dried to obtain a finished product of white carbon black, a potassium fluoride solution is discharged into a collecting tank to be concentrated and dried to obtain the finished product of potassium fluoride, the production efficiency of a process for preparing the potassium fluoride and co-producing the white carbon black by taking fluosilicic acid as a raw material is improved, and the production quality of the white carbon black is improved by controlling the reaction conditions.
Description
Technical Field
The invention belongs to the technical field of chemical technology, and relates to a process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material.
Background
The potassium fluoride is white monoclinic crystal or crystalline powder, has salty taste, is easy to absorb moisture, is soluble in water, is insoluble in ethanol, and is water-soluble
The liquid is alkaline, can corrode glass and porcelain, has a relative density of 2.454 and a melting point of 858 ℃; can be used for glass carving, food corrosion prevention, electroplating, soldering flux, pesticide, catalyst and absorbent (absorbing HF and moisture), and is used as an analysis reagent and a complex forming agent, and also is a raw material for preparing potassium hydrogen fluoride;
white carbon black is a generic term for white powder X-ray amorphous silicic acid and silicate products, mainly referring to precipitated silica, fumed silica and ultrafine silica gel, and also includes powder synthetic aluminum silicate, calcium silicate and the like.
The traditional method for preparing the white carbon black uses sodium silicate, silicon tetrachloride and tetraethoxysilane as silicon sources, and other cost is very high except sodium silicate, so that a process for preparing potassium fluoride and co-producing the white carbon black by taking fluosilicic acid as a raw material is designed to solve the problems.
Disclosure of Invention
Aiming at the problems, the invention provides a process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material, which aims at overcoming the defects of the prior art and comprises the following steps: the production efficiency of the process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material is conveniently improved, and the production quality of the white carbon black is improved by controlling the reaction conditions.
In order to achieve the above purpose, the technical scheme of the process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material provided by the invention is as follows: the method comprises the following steps:
step one: dissolving and filtering potassium chloride to obtain a potassium chloride solution, and placing the potassium chloride solution in a first reaction tank for standby;
step two: injecting the potassium chloride solution obtained in the first reaction tank in the first step into a reaction barrel to react with fluosilicic acid solution with the mass concentration of 30% -40%, wherein the pH of the reaction end point is 5-6, stirring for 25-35 min in the reaction barrel after the reaction is finished, and filtering and washing to obtain a potassium fluosilicate filter cake;
step three: adding the potassium fluosilicate filter cake obtained in the reaction barrel in the second step into water in a third reaction tank in proportion and stirring the water into paste to obtain potassium fluosilicate slurry, heating the potassium fluosilicate slurry in the reaction barrel to 60-80 ℃, then injecting 48% potassium hydroxide solution in the second reaction tank for reaction, wherein the reaction temperature in the reaction barrel is kept at 60-80 ℃, and the pH of the reaction end point is 7.5-8.5;
step four: after the reaction is completed, filtering the mixed slurry obtained in the step three reaction barrel to obtain a silicon dioxide filter cake and a filtrate containing potassium fluoride; washing and drying the silica filter cake to obtain a finished product of white carbon black; discharging the potassium fluoride solution into a collecting tank, concentrating the filtrate, and drying to obtain finished potassium fluoride;
still including installing the heating unit in the reaction barrel, install detecting element in the reaction barrel, the control unit is installed to the reaction barrel upside, install the display screen on the control unit, install drive assembly on the reaction barrel, drive assembly's output is fixed with the puddler, install four stirring boards on the puddler, wherein two stirring boards are fixed in on the puddler, two in addition the stirring board passes through the round bar and rotates to be installed on the puddler, install the adjusting part who is used for adjusting corresponding puddler angle in the puddler, be provided with filtration collection subassembly in the reaction barrel, filtration collection subassembly passes through first retort of pipeline subassembly intercommunication, second retort, third retort, collection tank and waste liquid jar, be provided with the conveying pipe on the reaction barrel.
Preferably, the drive assembly includes the first motor that is fixed in on the reaction barrel, be fixed with the backup pad in the reaction barrel, rotate in the backup pad and install two synchronizing wheels, two synchronizing wheels pass through the hold-in range and connect, one of them synchronizing wheel is fixed in the output of first motor, another synchronizing wheel is installed on the cooperation post, the puddler is fixed in on the cooperation post, the cooperation post slides and sets up on the synchronizing wheel that corresponds, cooperation post fixed mounting is on screw nut, screw nut meshes on reciprocating screw, reciprocating screw is fixed in the reaction barrel, be fixed with the quarter butt on the screw nut, the quarter butt slides and sets up in long section of thick bamboo, long section of thick bamboo is fixed in the swivel, the swivel rotates and sets up in the reaction barrel.
Preferably, the adjusting component comprises a second motor fixed in the stirring rod, a threaded rod is fixed at the output end of the second motor, a threaded cylinder is meshed on the threaded rod, a clamping block is fixed on the threaded cylinder, the threaded cylinder is arranged inside the stirring rod in a sliding mode through the clamping block, a rack is fixed on the threaded cylinder, two flat gears are meshed on the rack, and the two flat gears are both fixed on corresponding round rods.
Preferably, the stirring rod is rotatably provided with a connecting rod, a pressing plate is fixed on the connecting rod, and the stirring rod is arranged on the middle side plate in a sliding manner.
Preferably, the filter collecting assembly comprises a filter plate assembly arranged in the reaction barrel in a sliding manner, a supporting frame is fixed on the filter plate assembly, the supporting frame is fixed at the output end of a third motor through a long rod, the third motor is fixed at the output end of a first cylinder, a funnel shell is fixed at the lower part of the reaction barrel, a collecting shell is arranged at the lower part of the funnel shell in a sliding manner, the collecting shell is fixed at the output end of a second cylinder, and the collecting shell is communicated with a first reaction tank, a second reaction tank, a third reaction tank, a collecting tank and a waste liquid tank through pipeline assemblies.
Preferably, the filter plate assembly comprises a second partition plate fixed on the support frame, a first partition plate is rotatably arranged on the second partition plate, a filter plate is rotatably arranged on the first partition plate, the filter plate is slidably arranged on the reaction barrel, a vertical rod is fixed on the second partition plate, a vertical hole is formed in the first partition plate, and the second partition plate is connected with the first partition plate through the cooperation of the vertical rod and the vertical hole.
Preferably, the pipeline assembly comprises a waste liquid pipe communicated with the collecting shell, the waste liquid pipe is communicated with the waste liquid tank and the collecting pipe, the collecting pipe is communicated with the collecting tank and the air pressure pipe, the air pressure pipe is communicated with three connecting pipes, the three connecting pipes are respectively communicated with the first reaction tank, the second reaction tank and the third reaction tank, the first reaction tank, the second reaction tank and the third reaction tank are respectively communicated with the reaction tank through a liquid outlet pipe, each liquid outlet pipe is internally provided with a one-way valve, and electric regulating valves are respectively arranged between the waste liquid tank and the collecting pipe, between the collecting pipe and the air pressure pipe and between the air pressure pipe and the three connecting pipes.
Preferably, the inner side wall of the reaction barrel is provided with a ventilation pipeline.
Preferably, the heating unit comprises a heating shell fixed on the inner side wall of the reaction barrel, and an electric heating wire is arranged in the heating shell.
The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material has the following beneficial effects compared with the prior art:
1. the invention can observe the reaction condition of the solution in the reaction barrel in real time through the heating unit, the detection unit, the control unit and the display screen, and then control the temperature and the PH value in the reaction barrel.
2. According to the invention, through the mutual matching of the driving component, the stirring rod, the stirring plate, the filtering and collecting component and the adjusting component, the solution can be fully stirred, the reaction solution is added into the reaction barrel at a constant speed under control, the filtering and mixing efficiency of the reaction solution is improved, and the production quality is improved.
3. According to the invention, through the mutual matching of the pipeline assembly, the first reaction tank, the second reaction tank, the third reaction tank, the collecting tank and the waste liquid tank, the addition and the discharge in the reaction barrel are conveniently controlled.
4. The invention can complete the process of preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material, and can complete a plurality of processes by a monomer device, thereby improving the production efficiency.
Drawings
FIG. 1 is a schematic front view of the structure of the present invention;
FIG. 2 is a schematic view of the position of a stirring rod according to the present invention;
FIG. 3 is a schematic view of the position of a second separator according to the present invention;
FIG. 4 is a schematic view of a portion of the mating post and synchronizing wheel mating structure of the present invention;
FIG. 5 is a schematic illustration of the mating relationship between a filter plate assembly and a stirring rod of the present invention;
reference numerals: 1-first reaction tank, 2-reaction tank, 3-third reaction tank, 4-second reaction tank, 5-collection tank, 6-stirring rod, 7-stirring plate, 8-round rod, 9-waste liquid tank, 10-first motor, 11-support plate, 12-synchronizing wheel, 13-synchronous belt, 14-mating column, 15-lead screw nut, 16-reciprocating lead screw, 17-short rod, 18-long cylinder, 19-swivel, 20-second motor, 21-threaded rod, 22-threaded cylinder, 23-fixture block, 24-rack, 25-flat gear, 26-pressing plate, 27-connecting rod, 28-middle side plate, 29-support frame, 30-long rod, 31-third motor, 32-first cylinder, 33-funnel shell, 34-collection shell, 35-second partition plate, 36-first partition plate, 37-filter plate, 38-vertical rod, 39-vertical hole, 40-waste liquid pipe, 41-collection pipe, 42-pneumatic pipe, 43-44-electric control valve, 45-pipe, 46-vertical rod, 46-heating shell, 48-second air cylinder, 48-ventilation pipe.
Detailed Description
The following description of the embodiments of the present invention will be made clearly and completely with reference to the accompanying drawings, in which it is apparent that the embodiments described are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The following describes embodiments of the present invention in further detail with reference to FIGS. 1-5.
A process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material is shown in figures 1-3, and comprises the following steps:
step one: dissolving and filtering potassium chloride to obtain a potassium chloride solution, and placing the potassium chloride solution in a first reaction tank 1 for standby;
step two: injecting the potassium chloride solution obtained in the first reaction tank 1 in the first step into a reaction barrel 2 to react with fluosilicic acid solution with the mass concentration of 30% -40%, wherein the pH of the reaction end point is 5-6, stirring for 25-35 min in the reaction barrel 2 after the reaction is finished, and filtering and washing to obtain a potassium fluosilicate filter cake;
step three: adding water in a third reaction tank 3 into a potassium fluosilicate filter cake obtained in the reaction tank 2 in the second step in proportion, stirring into paste to obtain potassium fluosilicate slurry, heating the potassium fluosilicate slurry in the reaction tank 2 to 60-80 ℃, then injecting 48% potassium hydroxide solution in the second reaction tank 4 into the potassium fluosilicate slurry for reaction, and keeping the reaction temperature in the reaction tank 2 at 60-80 ℃ and the pH of the reaction end point at 7.5-8.5;
step four: after the reaction is completed, filtering the mixed slurry obtained in the reaction barrel 2 in the step three to obtain a silicon dioxide filter cake and a filtrate containing potassium fluoride; washing and drying the silica filter cake to obtain a finished product of white carbon black; discharging the potassium fluoride solution into a collecting tank 5, concentrating the filtrate, and drying to obtain finished potassium fluoride;
the reaction tank is characterized by further comprising a heating unit arranged in the reaction tank 2, a detection unit is arranged in the reaction tank 2, a control unit is arranged on the upper side of the reaction tank 2, a display screen is arranged on the control unit, a driving component is arranged on the reaction tank 2, a stirring rod 6 is fixed at the output end of the driving component, four stirring plates 7 are arranged on the stirring rod 6, two stirring plates 7 are fixed on the stirring rod 6, the other two stirring plates 7 are rotatably arranged on the stirring rod 6 through a round rod 8, an adjusting component for adjusting the angle of the corresponding stirring rod 6 is arranged in the stirring rod 6, a filtering collecting component is arranged in the reaction tank 2 and is communicated with a first reaction tank 1, a second reaction tank 4, a third reaction tank 3, a collecting tank 5 and a waste liquid tank 9 through pipeline components, and a feeding pipe is arranged on the reaction tank 2;
the detection unit comprises a PH meter and a thermometer and is used for detecting the PH value and the reaction temperature of the reaction solution;
the control unit can be a controller with model number FX1N-10MR and is used for controlling, analyzing and calculating information of other units and devices, and the control unit is connected with the devices and the units through wires;
firstly, dissolving and filtering potassium chloride, then placing the solution into a first reaction tank 1, adding fluosilicic acid solution with the mass concentration of 30% -40% into a reaction tank 2 through a feed pipe, then uniformly adding the potassium chloride solution in the first reaction tank 1 into the reaction tank 2 through a driving component, a stirring rod 6, a filtering and collecting component and a pipeline component, then driving the stirring rod 6 and a stirring plate 7 through the driving component to rotate so as to promote the reaction in the reaction tank 2, stopping the reaction when the PH of the solution in the reaction tank 2 is detected to be 5-6 through a detection unit, then filtering the solution into a waste liquid tank 9 through the filtering and collecting component and the pipeline component, adding water in a third reaction tank 3 into the reaction tank 2, then stirring and washing again through the stirring rod 6 and the stirring plate 7, filtering and discharging the solution to obtain a potassium fluosilicate filter cake, adding water in a third reaction tank 3 into a reaction tank 2 in proportion, stirring the solution in the reaction tank 2 to form paste to obtain potassium fluosilicate slurry, heating the potassium fluosilicate slurry in the reaction tank 2 to 60-80 ℃ by a heating unit, then injecting 48% potassium hydroxide solution into a second reaction tank 4 for stirring reaction, keeping the reaction temperature in the reaction tank 2 at 60-80 ℃ and the pH at the reaction end point at 7.5-8.5, filtering the mixed slurry obtained in the reaction tank 2 after the reaction is completed to obtain a silica filter cake and a filtrate containing potassium fluoride, extruding and filtering the silica filter cake in the reaction tank 2 by the cooperation of a filtering and collecting component, a stirring rod 6, a driving component and a pipeline component, putting the solution containing potassium fluoride into a collecting tank 5, washing the silica filter cake by water, and discharging waste liquid into a waste liquid tank 9, drying the silica filter cake by a heating unit to obtain a finished product of white carbon black, and taking out the finished product of white carbon black by opening a discharging door; and discharging the potassium fluoride solution into a filtrate in a collecting tank 5, taking out, concentrating and drying to obtain the finished potassium fluoride.
In this embodiment, as shown in fig. 1-4, the driving assembly includes a first motor 10 fixed on a reaction barrel 2, a supporting plate 11 is fixed in the reaction barrel 2, two synchronizing wheels 12 are rotatably installed on the supporting plate 11, the two synchronizing wheels 12 are connected through a synchronous belt 13, one synchronizing wheel 12 is fixed on an output end of the first motor 10, the other synchronizing wheel 12 is installed on a matching post 14, the stirring rod 6 is fixed on the matching post 14, the matching post 14 is slidably arranged on the corresponding synchronizing wheel 12, a matching block is fixed on the matching post 14, a tooth hole is formed on the synchronizing wheel 12, the cross section of the tooth hole is the same as the cross section of the matching post 14 matched with the matching block, the matching post 14 and the matching block can be slidably arranged on the synchronizing wheel 12 through the tooth hole, the matching post 14 is fixedly installed on a lead screw nut 15, the lead screw nut 15 is meshed on a reciprocating lead screw nut 16, the reciprocating screw 16 is fixed in the reaction barrel 2, a short nut 17 is fixed on the short nut 15, the short lead screw 17 is arranged on a long lead screw 18, and a long lead screw 19 is arranged in the reaction barrel 19;
the first motor 10 operates to drive the corresponding synchronizing wheel 12 to rotate, the synchronizing wheel 12 drives the other synchronizing wheel 12 to rotate through the synchronous belt 13, the other synchronizing wheel 12 rotates to drive the matched column 14 to rotate, the matched column 14 drives the screw nut 15 to rotate, at the moment, the screw nut 15 rotates and moves up and down along the reciprocating screw 16 to drive the matched column 14 to reciprocate up and down, when the screw nut 15 ascends, the short rod 17 is driven to move towards the long barrel 18, the short rod 17 stretches into the long barrel 18, when the screw nut 15 descends, the short rod 17 is driven to move out of the long barrel 18, the long barrel 18 is rotatably mounted on the inner side wall on the reaction barrel 2 through the swivel 19, when the matched column 14 rotates and reciprocates up and down, the matched column 14 drives the stirring rod 6 to reciprocate up and down and rotate, the stirring rod 6 is convenient to drive the stirring plate 7 to stir in the reaction barrel 2, and the reaction efficiency in the reaction barrel 2 is accelerated.
In this embodiment, as shown in fig. 2-3, the adjusting component includes a second motor 20 fixed in the stirring rod 6, the output end of the second motor 20 is fixed with a threaded rod 21, a threaded cylinder 22 is meshed with the threaded rod 21, a fixture block 23 is fixed on the threaded cylinder 22, the threaded cylinder 22 is slidably disposed in the stirring rod 6 through the fixture block 23, a rack 24 is fixed on the threaded cylinder 22, two flat gears 25 are meshed with the rack 24, the two flat gears 25 are both fixed on corresponding round rods 8, when the solution in the reaction barrel 2 needs to be filtered and extruded, the second motor 20 can be controlled to operate, the second motor 20 drives the threaded rod 21 to rotate, the threaded rod 21 drives the threaded cylinder 22 to move, the threaded cylinder 22 drives the fixture block 23 to slide, a chute is formed on the inner wall of the stirring rod 6, the threaded cylinder 22 can only move in the up-down direction through the fixture block 23, the rack 24 is driven to move, and the rack 24 is driven to rotate by the movement of the flat gears 25; when the solution in the reaction barrel 2 needs to be stirred, stirring is carried out by rotation through a stirring rod 6 and a stirring plate 7; when the solution in the reaction barrel 2 is required to be filtered and extruded, the stirring plate 7 and the round rod 8 are driven to rotate through the rack 24, and then the stirring plate 7 is matched with the filtering and collecting assembly to extrude and filter the solution, so that the filtering effect of the solution is improved, and the production quality is improved.
In this embodiment, as shown in fig. 2-3 and fig. 5, the stirring rod 6 is rotatably provided with a connecting rod 27, the stirring rod 6 is provided with a bearing, the connecting rod 27 is fixed on the bearing, the connecting rod 27 is rotatably provided on the stirring rod 6 through the bearing, the connecting rod 27 is fixedly provided with a pressing plate 26, the cross section of the pressing plate 26 is the same as the cross section of the upper narrow opening of the collecting shell 34, the stirring rod 6 is slidably arranged on the middle side plate 28, and the pressing plate 26 is driven to reciprocate up and down when the stirring rod 6 reciprocates up and down.
In this embodiment, as shown in fig. 2-3 and fig. 5, the filtering and collecting assembly includes a filter plate assembly slidably disposed in the reaction tank 2, a support frame 29 is fixed on the filter plate assembly, the support frame 29 is fixed at an output end of a third motor 31 through a long rod 30, the third motor 31 is fixed at an output end of a first cylinder 32, a funnel shell 33 is fixed at a lower portion of the reaction tank 2, a collecting shell 34 is slidably disposed at a lower portion of the funnel shell 33, the collecting shell 34 is fixed at an output end of a second cylinder 48, the collecting shell 34 adopts a design with narrow ends and wide middle, the collecting shell 34 is communicated with the first reaction tank 1, the second reaction tank 4, the third reaction tank 3, the collecting tank 5 and the waste liquid tank 9 through a pipeline assembly, the first cylinder 32 operates to drive the third motor 31 to move up and down, the third motor 31 operates to drive the support frame 29 to rotate, the support frame 29 drives the filter plate assembly to rotate, and the pressing plate 26 is mounted in the collecting shell 34.
In this embodiment, as shown in fig. 2-3, the filter plate assembly includes a second partition 35 fixed on the support 29, a first partition 36 is rotatably disposed on the second partition 35, a snap ring is disposed on an edge of the first partition 36, a clamping groove matched with the snap ring may be disposed on an inner wall of the reaction barrel 2, the first partition 36 may move up and down along the inner wall of the reaction barrel 2 through cooperation of the snap ring and the clamping groove, a filter plate 37 is rotatably disposed on the first partition 36, the filter plate 37 is slidably disposed on the reaction barrel 2, the first partition 36, the second partition 35 and the filter plate 37 are each composed of a plurality of blades equidistantly surrounding a central shaft of the stirring rod 6, a vertical rod 38 is fixed on the second partition 35, a vertical hole 39 is formed on the first partition 36, the second partition 35 is connected with the first partition 36 through cooperation of the vertical rod 38 and the vertical hole 39, when the first partition plate 36 cannot move downwards, the second partition plate 35 can move downwards continuously and is separated from the first partition plate 36, when the first partition plate 36 and the second partition plate 35 are matched with each other through the vertical holes 39 and the vertical rods 38, the support frame 29 drives the second partition plate 35 to rotate, the second partition plate 35 simultaneously drives the first partition plate 36 to rotate, when the second partition plate 35 is separated from the first partition plate 36, the support frame 29 only drives the second partition plate 35 to rotate, when the solution in the reaction barrel 2 is subjected to stirring reaction, the second partition plate 35 is matched with the first partition plate 36 to isolate the reaction barrel 2 from the collection shell 34, so that the reaction barrel 2 and the collection shell 34 cannot be communicated, at the moment, the solution in the reaction barrel 2 can be subjected to stirring reaction and cannot be filtered, when the second partition plate 35 is independently rotated, the filter plate 37 is communicated with the reaction barrel 2 and the collection shell 34, at the moment, the solution in the reaction barrel 2 can be filtered, when the second partition plate 35 rotates first to be flush with the first partition plate 36 and is matched with the first partition plate 36, the first partition plate 36 is driven to rotate, so that when the filter plates 37, the first partition plate 36 and the second partition plate 35 are aligned, filtered filter cakes in the reaction barrel 2 can enter the collecting shell 34 from the reaction barrel 2, solution or filter cakes entering the collecting shell 34 can enter the collecting tank 5 through the pipeline assembly, the stirring rod 6 penetrates through the second partition plate 35, the first partition plate 36 and the filter plates 37, and when the stirring rod 6 rotates or moves up and down, the second partition plate 35, the first partition plate 36 and the filter plates 37 are not driven to move.
In this embodiment, as shown in fig. 1-2, the pipeline assembly includes a waste liquid pipe 40 that is connected to the collecting shell 34, the waste liquid pipe 40 is connected to the waste liquid tank 9 and the collecting pipe 41, the collecting pipe 41 is connected to the collecting tank 5 and the air pressure pipe 42, the air pressure pipe 42 is connected to three connecting pipes 43, the three connecting pipes 43 are respectively connected to the first reaction tank 1, the second reaction tank 4 and the third reaction tank 3, the first reaction tank 1, the second reaction tank 4 and the third reaction tank 3 are all connected to the reaction tank 2 through liquid outlet pipes, a one-way valve is installed in each liquid outlet pipe 49, the liquid in each of the first reaction tank 1, the second reaction tank 4 and the third reaction tank 3 can only flow into the reaction tank 2, and an electric regulating valve 44 is arranged between the waste liquid tank 9 and the collecting pipe 41, between the collecting pipe 41 and the air pressure pipe 42 and between the air pressure pipe 42 and the three connecting pipes 43, and through the electric regulating valve 44, the connection between the waste liquid pipe 40, the collecting pipe 41, the air pressure pipe 42 and the air pressure pipe 43 can be controlled, wherein the collecting pipe 41 is inclined, and the filter cake is convenient for flowing out of the solution or the filter cake into the collecting tank 5.
In this embodiment, as shown in fig. 1-2, the inner side wall of the reaction tank 2 is provided with a ventilation pipeline 45, when the filter plate assembly isolates the communication relationship between the reaction tank 2 and the collecting shell 34, when the pressure plate 26 reciprocates up and down, air in the reaction tank 2 provides air to the collecting shell 34 through the ventilation pipeline 45 to stabilize the air pressure in the collecting shell 34, when the collecting shell 34 ascends through the second air cylinder 48, the pressure plate 26 enters a middle wide position from a narrow opening on the upper side of the collecting shell 34 when the pressure plate 26 exceeds half the position in the process of ascending through the second air cylinder 48, and at this time, the solution on the upper side of the pressure plate 26 in the collecting shell 34 can enter the lower side of the pressure plate 26 in the collecting shell 34, so that the solution enters the pipeline assembly, and when the collecting shell 34 descends through the second air cylinder 48, the pressure plate 26 moves to a position on the lowest side and is also located in the narrow opening of the collecting shell 34, so that the upper side inlet and the lower side outlet of the collecting shell 34 cannot be communicated.
In this embodiment, as shown in fig. 2-3, the heating unit includes a heating shell 46 fixed on the inner sidewall of the reaction tub 2, and an electric heating wire 47 is installed in the heating shell 46, and the reaction tub 2 is heated by the electric heating wire 47.
First, the first motor 10, the second motor 20, the third motor 31, the first cylinder 32, the second cylinder 48, the electric heating wire 47, and the detection unit are all connected to the control unit through wires.
The working process of the invention is as follows: firstly, dissolving and filtering potassium chloride, then placing the potassium chloride into a first reaction tank 1, adding fluosilicic acid solution with the mass concentration of 30% -40% into a reaction barrel 2 through a feed pipe, then driving a stirring rod 6 and a stirring plate 7 to reciprocate up and down and rotate through a control driving component, opening a collecting shell 34 to sequentially communicate a waste liquid tank 9, a collecting pipe 41, an air pressure pipe 42, a connecting pipe 43 and an electric regulating valve 44 in a path of the first reaction tank 1, pressing a first reaction tank 1 by up-down movement of a pressing plate 26, so that the potassium chloride solution is discharged into the reaction barrel 2 to react, driving the solution in the reaction barrel 2 to react through the stirring plate 7, closing the electric regulating valve 44 communicated with the first reaction tank 1 when a detection unit displays that the PH of the solution in the reaction barrel 2 is 5% -6, driving the collecting shell 34 to ascend through a second cylinder 48, driving the second partition 35 to descend through the first cylinder 32, at this time, the second partition 35 and the first partition 36 are separated, then the third motor 31 drives the second partition 35 to rotate, the solution in the reaction barrel 2 is filtered through the filter plate 37, at this time, the stirring plate 7 continuously rotates, the pressing plate 26 moves up and down in a reciprocating manner, when the pressing plate 26 moves down and is separated from the narrow opening on the collecting shell 34, the solution flows into the pipeline assembly from the collecting shell 34 each time, the waste liquid flows into the waste liquid tank 9 through controlling the electric regulating valve 44 of the waste liquid pipe 40 to be communicated with the waste liquid tank 9, then the third motor 31 and the first air cylinder 32 are controlled to drive the second partition 35 to reset, the second air cylinder 48 drives the collecting shell 34 to reset, at this time, the pressing plate 26 continuously extrudes the inside of the collecting shell 34 when moving up and down, at this time, the electric regulating valve 44 of the third reaction tank 3 with water is opened to enable the water to enter the reaction barrel 2 to be stirred and washed, the washing is connected, the electric regulating valve 44 of the third reaction tank 3 is closed, the waste liquid tank 9 is communicated, the waste liquid is discharged, the reaction barrel 2 and the collecting shell 34 are closed at the moment, then the electric regulating valve 44 communicated with the third reaction tank 3 is opened, the second motor 20 is controlled to operate to drive the stirring plate 7 to rotate, the wider side of the stirring plate 7 is enabled to be horizontal to the filter plate 37, meanwhile, the first cylinder 32 is controlled to drive the filter plate assembly to ascend, the stirring plate 7 is enabled to be attached to the filter plate 37 when the stirring plate 7 is lowered to the lowest position, at the moment, the stirring plate 7 continuously rotates, the pressing plate 26 extrudes and drives the solution in the third reaction tank 3 to be added into the reaction barrel 2, at the moment, the stirring plate 7 continuously hits the filter cake in the reaction barrel 2, stirring is carried out, the filter cake is enabled to be rapidly stirred into paste, the filter cake can be fully dispersed and fused into the solution through beating, the electric regulating valve 44 of the third reaction tank 3 is closed, after the potassium fluosilicate slurry in the reaction barrel 2 is heated to 60-80 ℃ through the heating unit, an electric regulating valve 44 of a second reaction tank 4 is opened to inject 48% potassium hydroxide solution into the second reaction tank 4 for reaction, the reaction temperature in the reaction barrel 2 is kept at 60-80 ℃, the pH of the reaction end point is 7.5-8.5, the electric regulating valve 44 of the second reaction tank 4 is closed after the reaction is finished, an electric regulating valve 44 of a collecting tank 5 is opened, a first cylinder 32 and a third motor 31 are controlled to drive a second partition 35 to rotate downwards, the second partition 35 is exposed out of a filter plate 37 and aligned with the first partition 36, at the moment, a silica filter cake is continuously beaten through a stirring plate 7, so that potassium chloride solution in the silica filter cake is discharged, after the potassium chloride solution is discharged, the second partition 35 is aligned with the filter plate 37, the reaction barrel 2 and the collecting shell 34 are sealed, and the third reaction tank 3 is communicated, water is added, stirring and washing are carried out, then waste liquid is discharged, and then heating and drying are carried out through a heating unit, at the moment, the potassium fluoride solution is taken out, concentrated and dried to obtain finished product potassium fluoride, and the dried finished product white carbon black in the reaction barrel 2 is discharged into an empty collection tank 5.
Although the present invention has been described with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments described, or equivalents may be substituted for elements thereof, and any modifications, equivalents, improvements and changes may be made without departing from the spirit and principles of the present invention.
Claims (7)
1. A process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material is characterized in that: the method comprises the following steps:
step one: dissolving and filtering potassium chloride to obtain a potassium chloride solution, and placing the potassium chloride solution in a first reaction tank for standby;
step two: injecting the potassium chloride solution obtained in the first reaction tank in the first step into a reaction barrel to react with fluosilicic acid solution with the mass concentration of 30% -40%, wherein the pH of the reaction end point is 5-6, stirring for 25-35 min in the reaction barrel after the reaction is finished, and filtering and washing to obtain a potassium fluosilicate filter cake;
step three: adding the potassium fluosilicate filter cake obtained in the reaction barrel in the second step into water in a third reaction tank in proportion and stirring the water into paste to obtain potassium fluosilicate slurry, heating the potassium fluosilicate slurry in the reaction barrel to 60-80 ℃, then injecting 48% potassium hydroxide solution in the second reaction tank for reaction, wherein the reaction temperature in the reaction barrel is kept at 60-80 ℃, and the pH of the reaction end point is 7.5-8.5;
step four: after the reaction is completed, filtering the mixed slurry obtained in the step three reaction barrel to obtain a silicon dioxide filter cake and a filtrate containing potassium fluoride; washing and drying the silica filter cake to obtain a finished product of white carbon black; discharging the potassium fluoride solution into a collecting tank, concentrating the filtrate, and drying to obtain finished potassium fluoride;
the device comprises a reaction barrel, and is characterized by further comprising a heating unit arranged in the reaction barrel, wherein a detection unit is arranged in the reaction barrel, a control unit is arranged beside the reaction barrel, a display screen is arranged on the control unit, a driving assembly is arranged on the reaction barrel, the output end of the driving assembly is fixedly provided with a stirring rod, four stirring plates are arranged on the stirring rod, two stirring plates are fixedly arranged on the stirring rod, the other two stirring plates are rotatably arranged on the stirring rod through a round rod, an adjusting assembly for adjusting the angle of the corresponding stirring rod is arranged in the stirring rod, a filtering and collecting assembly is arranged in the reaction barrel and communicated with a first reaction tank, a second reaction tank, a third reaction tank, a collecting tank and a waste liquid tank through pipeline assemblies, and a feeding pipe is arranged on the reaction barrel;
the filtering and collecting assembly comprises a filter plate assembly which is arranged in the reaction barrel in a sliding manner, a supporting frame is fixed on the filter plate assembly, the supporting frame is fixed at the output end of a third motor through a long rod, the third motor is fixed at the output end of a first cylinder, a funnel shell is fixed at the lower part of the reaction barrel, a collecting shell is arranged at the lower part of the funnel shell in a sliding manner, the collecting shell is fixed at the output end of a second cylinder, and the collecting shell is communicated with a first reaction tank, a second reaction tank, a third reaction tank, a collecting tank and a waste liquid tank through pipeline assemblies;
the filter plate assembly comprises a second partition plate fixed on a supporting frame, a first partition plate is rotatably arranged on the second partition plate, a filter plate is rotatably arranged on the first partition plate, the filter plate is slidably arranged on a reaction barrel, a vertical rod is fixed on the second partition plate, a vertical hole is formed in the first partition plate, and the second partition plate is connected with the first partition plate through the cooperation of the vertical rod and the vertical hole.
2. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: the driving assembly comprises a first motor fixed on the reaction barrel, a supporting plate is fixed in the reaction barrel, two synchronous wheels are rotatably arranged on the supporting plate and connected through a synchronous belt, one synchronous wheel is fixed at the output end of the first motor, the other synchronous wheel is arranged on a matching column, a stirring rod is fixed on the matching column, the matching column is slidably arranged on the corresponding synchronous wheel, the matching column is fixedly arranged on a screw nut, the screw nut is meshed on a reciprocating screw, the reciprocating screw is fixed in the reaction barrel, a short rod is fixed on the screw nut, the short rod is slidably arranged in a long barrel, the long barrel is fixed on a rotating ring, and the rotating ring is rotatably arranged in the reaction barrel.
3. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: the adjusting component comprises a second motor fixed in the stirring rod, a threaded rod is fixed at the output end of the second motor, a threaded cylinder is meshed with the threaded rod, a clamping block is fixed on the threaded cylinder, the threaded cylinder is arranged inside the stirring rod in a sliding mode through the clamping block, a rack is fixed on the threaded cylinder, two flat gears are meshed on the rack, and the two flat gears are fixed on corresponding round rods.
4. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: the stirring rod is rotatably provided with a connecting rod, a pressing plate is fixed on the connecting rod, and the stirring rod is arranged on the middle side plate in a sliding manner.
5. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: the pipeline subassembly is including the waste liquid pipe of intercommunication collection shell, waste liquid pipe intercommunication waste liquid jar and collecting pipe, collecting pipe intercommunication collecting tank and pneumatic tube, pneumatic tube intercommunication has three connecting pipe, and is three the connecting pipe communicates first retort, second retort and third retort respectively, first retort, second retort and third retort all communicate the reaction vessel through the drain pipe, every all install the check valve in the drain pipe, all be equipped with electric control valve between waste liquid jar and the collecting pipe, between collecting pipe and the pneumatic tube and between pneumatic tube and the three connecting pipe.
6. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: and a ventilation pipeline is arranged on the inner side wall of the reaction barrel.
7. The process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as a raw material according to claim 1, which is characterized in that: the heating unit comprises a heating shell fixed on the inner side wall of the reaction barrel, and an electric heating wire is arranged in the heating shell.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410288246.7A CN117886335A (en) | 2024-03-14 | 2024-03-14 | Process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as raw material |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202410288246.7A CN117886335A (en) | 2024-03-14 | 2024-03-14 | Process for preparing potassium fluoride and co-producing white carbon black by taking fluosilicic acid as raw material |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101954222A (en) * | 2010-09-25 | 2011-01-26 | 石家庄波特无机膜分离设备有限公司 | Filtering and washing device |
| CN208927728U (en) * | 2018-05-31 | 2019-06-04 | 浙江省天正设计工程有限公司 | It is a kind of to integrate the three-in-one device be separated by filtration, wash, drying |
| CN110510640A (en) * | 2019-10-08 | 2019-11-29 | 内蒙古星汉氟都化工有限公司 | A method of it with fluosilicic acid is that raw material prepares potassium fluoride co-producing white carbon black |
| CN114853044A (en) * | 2022-05-12 | 2022-08-05 | 广西南宁百会药业集团有限公司 | Production system of hydrotalcite |
-
2024
- 2024-03-14 CN CN202410288246.7A patent/CN117886335A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101954222A (en) * | 2010-09-25 | 2011-01-26 | 石家庄波特无机膜分离设备有限公司 | Filtering and washing device |
| CN208927728U (en) * | 2018-05-31 | 2019-06-04 | 浙江省天正设计工程有限公司 | It is a kind of to integrate the three-in-one device be separated by filtration, wash, drying |
| CN110510640A (en) * | 2019-10-08 | 2019-11-29 | 内蒙古星汉氟都化工有限公司 | A method of it with fluosilicic acid is that raw material prepares potassium fluoride co-producing white carbon black |
| CN114853044A (en) * | 2022-05-12 | 2022-08-05 | 广西南宁百会药业集团有限公司 | Production system of hydrotalcite |
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