CN115403013B - Preparation method and preparation device of ammonium persulfate crystals - Google Patents
Preparation method and preparation device of ammonium persulfate crystals Download PDFInfo
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- CN115403013B CN115403013B CN202211054552.1A CN202211054552A CN115403013B CN 115403013 B CN115403013 B CN 115403013B CN 202211054552 A CN202211054552 A CN 202211054552A CN 115403013 B CN115403013 B CN 115403013B
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- ammonium persulfate
- fixedly connected
- plate
- dryer
- compression
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- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 title claims abstract description 315
- 229910001870 ammonium persulfate Inorganic materials 0.000 title claims abstract description 159
- 239000013078 crystal Substances 0.000 title claims abstract description 67
- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 238000001035 drying Methods 0.000 claims abstract description 31
- 238000000034 method Methods 0.000 claims abstract description 26
- 230000008569 process Effects 0.000 claims abstract description 19
- 230000006835 compression Effects 0.000 claims description 71
- 238000007906 compression Methods 0.000 claims description 71
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 claims description 32
- 229910052921 ammonium sulfate Inorganic materials 0.000 claims description 32
- 235000011130 ammonium sulphate Nutrition 0.000 claims description 32
- 238000002425 crystallisation Methods 0.000 claims description 27
- 230000008025 crystallization Effects 0.000 claims description 27
- 239000006185 dispersion Substances 0.000 claims description 16
- 239000007788 liquid Substances 0.000 claims description 16
- 238000007790 scraping Methods 0.000 claims description 16
- 238000003825 pressing Methods 0.000 claims description 14
- 239000007787 solid Substances 0.000 claims description 14
- 238000001816 cooling Methods 0.000 claims description 12
- 239000000203 mixture Substances 0.000 claims description 12
- 239000002245 particle Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 238000001125 extrusion Methods 0.000 claims description 7
- 238000010438 heat treatment Methods 0.000 claims description 6
- 238000003756 stirring Methods 0.000 claims description 6
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 claims description 5
- -1 ammonium persulfate ions Chemical class 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 3
- 150000002500 ions Chemical class 0.000 claims description 3
- 230000009471 action Effects 0.000 description 7
- 230000001276 controlling effect Effects 0.000 description 6
- 238000005096 rolling process Methods 0.000 description 4
- 238000004519 manufacturing process Methods 0.000 description 3
- 230000007246 mechanism Effects 0.000 description 2
- 238000006116 polymerization reaction Methods 0.000 description 2
- 230000009467 reduction Effects 0.000 description 2
- 230000001105 regulatory effect Effects 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- BZHJMEDXRYGGRV-UHFFFAOYSA-N Vinyl chloride Chemical class ClC=C BZHJMEDXRYGGRV-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000006460 hydrolysis reaction Methods 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010899 nucleation Methods 0.000 description 1
- 230000006911 nucleation Effects 0.000 description 1
- 239000007800 oxidant agent Substances 0.000 description 1
- 239000003208 petroleum Substances 0.000 description 1
- 239000012985 polymerization agent Substances 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- GGCZERPQGJTIQP-UHFFFAOYSA-N sodium;9,10-dioxoanthracene-2-sulfonic acid Chemical compound [Na+].C1=CC=C2C(=O)C3=CC(S(=O)(=O)O)=CC=C3C(=O)C2=C1 GGCZERPQGJTIQP-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B15/00—Peroxides; Peroxyhydrates; Peroxyacids or salts thereof; Superoxides; Ozonides
- C01B15/055—Peroxyhydrates; Peroxyacids or salts thereof
- C01B15/06—Peroxyhydrates; Peroxyacids or salts thereof containing sulfur
- C01B15/08—Peroxysulfates
Abstract
The invention belongs to the technical field of ammonium persulfate preparation, in particular to a preparation method and a preparation device of ammonium persulfate crystals, wherein the outer surface of a dryer is fixedly connected with a conveying pipeline; the outer surface of the conveying pipeline is rotatably connected with a rotating wheel; the rotating wheel is connected with the output end of the external motor; the outer surface of the rotating wheel is fixedly connected with a first connecting rod; the surface of the first connecting rod is rotationally connected with a second connecting rod; one end of the second connecting rod far away from the first connecting rod is rotatably connected with a conveying plate; the width of the conveying plate is matched with the width of the conveying pipeline; the conveying plate can be in contact with the dispersing plate in the moving process of the conveying pipeline, and certain pressure is given to the dispersing plate, so that the dispersing plate is in an open state with a certain amplitude, and the dispersing plate separates the ammonium persulfate bonded together, so that the problem that the ammonium persulfate is easy to bond together due to the fact that the ammonium persulfate is high in humidity in the prior art is solved, and drying is facilitated later.
Description
Technical Field
The invention belongs to the technical field of ammonium persulfate preparation, and particularly relates to a preparation method and a preparation device of ammonium persulfate crystals.
Background
Ammonium persulfate is colorless monoclinic crystal or white powdery crystal, is easy to dissolve in water, and has high solubility in warm water; the dry ammonium persulfate has good stability and is easy to be damp and agglomerate in moist air; after the ammonium persulfate absorbs moisture, hydrolysis reaction can occur in the aqueous solution; can be oxidized and decomposed under the catalysis of substances such as silver salt and the like, and emits a large amount of heat energy.
Ammonium persulfate has wide application in the fields of chemical industry, light industry, electronics, petroleum, food industry and the like; mainly used as an oxidizing agent, a polymerization accelerator for high molecular polymerization, a polymerization agent for vinyl chloride compounds, etc., and therefore, is also important in the preparation of ammonium persulfate crystals.
In the prior art, when ammonium persulfate is used for producing crystals, direct and rapid cooling is generally adopted to obtain a crystal product, but the direct cooling method ensures that the crystals are not easy to nucleate, the nucleation granularity is uneven, a large number of small crystals are generated, and moisture absorption and agglomeration of the ammonium persulfate are possibly caused, so that the use of the crystals is not facilitated.
Therefore, the invention provides a preparation method and a preparation device of ammonium persulfate crystals.
Disclosure of Invention
In order to overcome the deficiencies of the prior art, at least one technical problem presented in the background art is solved.
The technical scheme adopted for solving the technical problems is as follows: the preparation method of ammonium persulfate crystals provided by the invention comprises the following steps:
s1, proportioning: firstly, introducing ammonium persulfate into a batching box, adding ammonium sulfate in the batching process, stirring while adding the ammonium sulfate, wherein the stirring speed is 30-40r/min, so that the ammonium sulfate and the ammonium persulfate are fully dissolved to obtain a mixed material liquid of the ammonium persulfate and the ammonium sulfate, then introducing ammonia gas to enable the pH value to be 5.0-7.0, wherein the concentration of ammonium persulfate ions in the mixed material liquid is 0.35-0.45g/mL, and the ion concentration of the ammonium sulfate is 0.62-1.2g/mL;
s2, crystallizing: introducing ammonium persulfate and ammonium sulfate mixed feed liquid into a crystallization tank, controlling the temperature of the mixed feed liquid to be maintained at 28-35 ℃, adding ammonium persulfate finished products with the particle size of 30-40 meshes as seed crystals, slowly heating to 0.6-0.8 ℃, and then cooling to-4-6 ℃ at a cooling rate of 8-10 ℃/h for crystallization to obtain a crystallization mixture;
s3, drying: filtering the obtained crystallization mixture to obtain a solid, and introducing the obtained wet solid into a dryer for drying to obtain ammonium persulfate crystals. .
In the crystallization process, the use of ammonium persulfate crystal seeds is reduced, the temperature reduction speed is controlled sequentially by slowly heating up to a certain extent, the granularity of the manufactured crystal is increased and uniform by the cooperation of multiple factors, the production and crystallization process of the crystal can be controlled better, the purity, uniformity and average particle size of the crystal are improved, the generation of too small crystal is reduced, and the anti-caking property of the ammonium persulfate crystal can be improved
Preferably, in the step S2, if the weight portion of the mixed solution of ammonium persulfate and ammonium sulfate is 8-12 portions, the adding amount of the ammonium persulfate seed crystal is 18-22 portions; by controlling the amount of the added seed crystal, the particle size of the finally obtained crystal is larger under the condition that the mass of the precipitated ammonium persulfate is the same, and the generation of excessively small crystal is reduced.
A preparation device of ammonium persulfate crystals, which is suitable for the preparation method of the ammonium persulfate crystals; the outer surface of the dryer is fixedly connected with a conveying pipeline; the outer surface of the conveying pipeline is rotatably connected with a rotating wheel; the rotating wheel is connected with the output end of the external motor; the outer surface of the rotating wheel is fixedly connected with a first connecting rod; the surface of the first connecting rod is rotationally connected with a second connecting rod; one end of the second connecting rod far away from the first connecting rod is rotatably connected with a conveying plate; the width of the conveying plate is matched with the width of the conveying pipeline; a plurality of turntables are rotatably connected in the conveying pipeline; a plurality of dispersing plates are arranged on the outer surface of each turntable; a feeding pipeline is fixedly connected inside the conveying pipeline; during operation, when the solid ammonium persulfate of wet product is introduced into the conveying pipeline through the feeding pipeline, the driving motor drives the rotating wheel and the first connecting rod to rotate, the first connecting rod drives the second connecting rod to rotate, the second connecting rod can transversely and circularly reciprocate to drive the conveying plate under the action of the first connecting rod and the second connecting rod, the conveying plate can continuously convey the solid wet product to the inside of the dryer, meanwhile, the conveying plate can be in contact with the dispersing plate in the moving process of the conveying pipeline, certain pressure is given to the dispersing plate, the dispersing plate is in an open state with a certain amplitude, the dispersing plate separates the ammonium persulfate bonded together, and the problem that the ammonium persulfate is easy to bond together due to the fact that the ammonium persulfate is high in humidity in the prior art is solved, and drying after the ammonium persulfate is convenient is facilitated.
Preferably, the outer surface of the dispersion plate is fixedly connected with an arc-shaped bulge; the outer surface of the dispersion plate is fixedly connected with an extension spring; the conveying plate is fixedly connected with symmetrically arranged pressing columns at one side close to the dispersing plate; the surface of each compression column is fixedly connected with a compression head; the compression head is semicircular in shape; the compression head and the arc-shaped bulge are arranged on the same axis; during operation, the conveying plate drives the compression column to move, the compression column can drive the compression head on the surface of the compression column to move simultaneously, the compression head can be in contact with and extrude with the arc-shaped protrusions on the surface of the dispersing plate in the moving process, the dispersing plate extrudes the tension spring and rotates at a certain angle, and when the arc-shaped protrusions are separated from the compression head, the dispersing plate and the tension spring are not extruded any more, so that the tension spring and the dispersing plate recover, and the dispersing plate extrudes the ammonium persulfate bonded together, so that the ammonium persulfate is dispersed.
Preferably, the number of the single compression heads on the surface of the compression column is multiple, and the compression heads are equidistantly arranged on the outer surface of the compression column; the diameter of the compression head is larger than that of the arc-shaped bulge; during operation, because the plurality of compression heads are arranged, the compression heads can intermittently contact with the arc-shaped bulges and extrude the arc-shaped bulges, so that the dispersing plate can intermittently rotate and recover, the dispersing speed of bonding ammonium persulfate is improved, and the drying of the ammonium persulfate is facilitated.
Preferably, a telescopic rod is fixedly connected to one side of the inner wall of the conveying pipeline, which is close to the dispersing plate; the outer surface of the telescopic rod is fixedly connected with a limit spring; one end of the telescopic rod, which is close to the dispersing plate, is fixedly connected with a scraping head; when the ammonium persulfate scraper works, the dispersing plate moves to one side close to the scraping head when being pressed to rotate, and then contacts and extrudes the scraping head, so that the scraping head drives the telescopic rod to move, the scraping head can scrape the ammonium persulfate adhered on the surface of the dispersing plate, and the dispersing plate is ensured to normally separate the ammonium persulfate.
Preferably, a drying fan is fixedly connected in the dryer; a cam shaft is rotatably connected to the interior of the dryer; the inside of the dryer is rotatably connected with a bearing plate; the bearing plate is arranged close to one side of the cam shaft; the lower surface of the bearing plate is fixedly connected with an extrusion spring on the inner wall of the dryer; it should be noted that, the camshaft is connected with the output end of the external motor, and the connection mode is the prior art, and redundant description is not made in this embodiment; when ammonium persulfate enters into the surface of the bearing plate inside the dryer through the conveying pipeline, hot air is blown into the dryer through the control drying fan, the ammonium persulfate is dried, meanwhile, the external motor drives the cam shaft to rotate, the cam shaft can be contacted with the lower surface of the bearing plate and extruded when rotating, so that the bearing plate is rotated at a certain angle, the bearing plate is inclined, when the cam shaft and the bearing plate are separated from each other, the bearing plate returns under the action of the extrusion spring, so that the ammonium persulfate on the surface of the bearing plate can roll continuously at a certain angle on the surface of the bearing plate, in the continuous rolling process, the hot air blown by the fan can dry different surfaces of the ammonium persulfate, the contact area between the ammonium persulfate and the hot air is improved, and the problem that the partially dark surface of the ammonium persulfate is difficult to dry in the prior art is solved.
Preferably, the inner part of the bearing plate is connected with an elastic post rod in a sliding way; the upper end of the elastic post rod is fixedly connected with a pressing block; a compression bag is fixedly connected to one side, close to the elastic post rod, of the inner part of the bearing plate; the outer surface of the compression bag is fixedly connected with an air outlet pipe; when the ammonium persulfate is driven to rotate by the bearing plate, the ammonium persulfate can simultaneously give a certain pressure to the pressing block in the bearing plate, so that the pressing block drives the elastic post rod to move, the elastic post rod can squeeze the compression bag, gas in the compression bag is squeezed out, and the gas is blown into the ammonium persulfate through the gas outlet pipe, so that the gas is completely contacted with the ammonium persulfate, and the drying efficiency of the ammonium persulfate is improved; the material of the compression bag is rubber, and the compression bag can be restored to the initial state when the compression bag is not stressed.
Preferably, the inside of the air outlet pipe is fixedly connected with a one-way valve; the air outlet pipe is obliquely arranged, and a one-way valve is arranged, so that the air can be blown in one direction.
Preferably, the inner wall of the dryer is fixedly connected with a hot air pipeline; the hot air pipeline is annularly arranged on the inner wall of the dryer; one end of the hot air pipeline is connected with the output end of the drying fan; the annular hot air pipeline can better enable hot air to be blown to the surface of the ammonium persulfate, and is convenient to dry the ammonium persulfate.
The beneficial effects of the invention are as follows:
1. according to the preparation method and the preparation device of the ammonium persulfate crystal, the use of ammonium persulfate crystal seeds is reduced in the crystallization process, the temperature reduction speed is controlled sequentially by slowly heating up to a certain extent, and the manufactured crystal granularity is increased and uniform through the cooperation of multiple factors, so that the production and crystallization process of the crystal can be controlled better, the increase of the crystal purity, the uniformity and the average particle size is improved, the generation of too small crystals is reduced, and the anti-caking performance of the ammonium persulfate crystal can be improved.
2. According to the preparation method and the preparation device of the ammonium persulfate crystals, the conveying plates are contacted with the dispersing plates in the process of moving in the conveying pipeline, and a certain pressure is applied to the dispersing plates, so that the dispersing plates are in a certain-amplitude open state, the dispersing plates separate the ammonium persulfate bonded together, the problem that the ammonium persulfate is easy to bond together due to high humidity of the ammonium persulfate in the prior art is solved, and the subsequent drying is facilitated.
3. According to the preparation method and the preparation device for the ammonium persulfate crystals, the bearing plate is rotated at a certain angle, so that the bearing plate is in an inclined state, when the cam shaft and the bearing plate are separated from each other, the bearing plate returns under the action of the extrusion spring, so that ammonium persulfate on the surface of the bearing plate can roll continuously at a certain angle, in the continuous rolling process, different surfaces of the ammonium persulfate can be dried by hot air blown by the fan, the contact area of the ammonium persulfate and the hot air is increased, and the problem that part of dark surfaces of the ammonium persulfate are difficult to dry in the prior art is solved.
Drawings
The invention is further described below with reference to the accompanying drawings.
FIG. 1 is a flow chart of the method of the present invention;
fig. 2 is a schematic perspective view of a dryer according to the present invention;
FIG. 3 is a cross-sectional view of a transfer conduit in accordance with the present invention;
FIG. 4 is an enlarged view of the structure of FIG. 3A in accordance with the present invention;
fig. 5 is a schematic cross-sectional structure of a dryer according to the present invention;
FIG. 6 is an enlarged view of the structure at B of FIG. 5 in accordance with the present invention;
fig. 7 is a schematic view of a hot air duct structure according to a second embodiment of the present invention.
In the figure: 1. a dryer; 2. a delivery conduit; 3. a rotating wheel; 4. a first link; 5. a second link; 6. a conveying plate; 7. a turntable; 8. a dispersion plate; 81. a tension spring; 9. arc-shaped bulges; 10. pressing a column; 11. a compression head; 12. a telescopic rod; 13. a limit spring; 14. a scraping head; 15. a drying fan; 16. a cam shaft; 17. a receiving plate; 18. extruding a spring; 19. an elastic post; 20. briquetting; 21. a compression bladder; 22. an air outlet pipe; 23. a one-way valve; 24. a hot air duct.
Detailed Description
The invention is further described in connection with the following detailed description in order to make the technical means, the creation characteristics, the achievement of the purpose and the effect of the invention easy to understand.
As shown in fig. 1 to 2, the preparation method of ammonium persulfate crystals according to the embodiment of the invention comprises the following steps:
s1, proportioning: firstly, introducing ammonium persulfate into a batching box, adding ammonium sulfate in the batching process, stirring while adding the ammonium sulfate, wherein the stirring speed is 30-40r/min, so that the ammonium sulfate and the ammonium persulfate are fully dissolved to obtain a mixed material liquid of the ammonium persulfate and the ammonium sulfate, then introducing ammonia gas to enable the pH value to be 5.0-7.0, wherein the concentration of ammonium persulfate ions in the mixed material liquid is 0.35-0.45g/mL, and the ion concentration of the ammonium sulfate is 0.62-1.2g/mL; the weight percentages of the raw materials are as follows: 38-56% of ammonium persulfate and the balance of ammonium sulfate.
S2, crystallizing: introducing ammonium persulfate and ammonium sulfate mixed feed liquid into a crystallization tank, controlling the temperature of the mixed feed liquid to be maintained at 28-35 ℃, adding ammonium persulfate finished products with the particle size of 30-40 meshes as seed crystals, slowly heating to 0.6-0.8 ℃, and then cooling to-4-6 ℃ at a cooling rate of 8-10 ℃/h for crystallization to obtain a crystallization mixture;
s3, drying: filtering the obtained crystallization mixture to obtain a solid, and introducing the obtained wet solid into a dryer 1 for drying to obtain a finished product of ammonium persulfate crystals.
In the crystallization process, the use of ammonium persulfate crystal seeds is reduced, the cooling speed is controlled sequentially by slowly heating up to a certain extent, and the manufactured crystal granularity is increased and uniform through the cooperation of multiple factors, so that the production and crystallization process of the crystal can be controlled better, the increase of the crystal purity, the uniformity and the average particle size is improved, the generation of too small crystals is reduced, and the anti-caking performance of the ammonium persulfate crystal can be improved.
In the step S2, calculated by the weight parts of the ammonium persulfate and ammonium sulfate mixed feed liquid, if the weight parts of the ammonium persulfate and ammonium sulfate mixed feed liquid are 8-12 parts, the adding amount of ammonium persulfate seed crystals is 18-22 parts; by controlling the amount of the added seed crystal, the particle size of the finally obtained crystal is larger under the condition that the mass of the precipitated ammonium persulfate is the same, and the generation of excessively small crystal is reduced.
A preparation device of ammonium persulfate crystals, which is suitable for the preparation method of the ammonium persulfate crystals; when the obtained wet solid matters are fed into a dryer for drying, the problem that the wet solid matters are easy to adhere together in the conveying process and influence the subsequent drying due to the fact that the humidity of part of the wet matters is high is solved; as shown in fig. 2 to 4, the outer surface of the dryer 1 is fixedly connected with a conveying pipeline 2; the outer surface of the conveying pipeline 2 is rotatably connected with a rotating wheel 3; the rotating wheel 3 is connected with the output end of an external motor; the outer surface of the rotating wheel 3 is fixedly connected with a first connecting rod 4; the surface of the first connecting rod 4 is rotatably connected with a second connecting rod 5; one end of the second connecting rod 5 far away from the first connecting rod 4 is rotatably connected with a conveying plate 6; the width of the conveying plate 6 is matched with the width of the conveying pipeline 2; a plurality of turntables 7 are rotatably connected in the conveying pipeline 2; the outer surface of each turntable 7 is provided with a plurality of dispersing plates 8; a feeding pipeline is fixedly connected inside the conveying pipeline 2; during operation, when the solid ammonium persulfate of wet products is introduced into the conveying pipeline 2 through the feeding pipeline, the driving motor drives the rotating wheel 3 and the first connecting rod 4 to rotate, the first connecting rod 4 drives the second connecting rod 5 to rotate, the second connecting rod 5 can transversely and circularly reciprocate to drive the conveying plate 6 under the action of the first connecting rod 4 and the second connecting rod 5, and then the conveying plate 6 can continuously convey the solid wet products to the inside of the dryer 1, meanwhile, the conveying plate 6 can be in contact with the dispersing plate 8 in the moving process of the conveying pipeline 2, and certain pressure is given to the dispersing plate 8, so that the dispersing plate 8 is in an open state with a certain amplitude, the dispersing plate 8 separates the ammonium persulfate bonded together, the problem that the ammonium persulfate is easy to bond together due to high ammonium persulfate humidity in the prior art is solved, and drying after that is convenient.
Wherein the outer surface of the dispersing plate 8 is fixedly connected with an arc-shaped bulge 9; the outer surface of the dispersion plate 8 is fixedly connected with an extension spring 81; the conveying plate 6 is fixedly connected with symmetrically arranged press columns 10 at one side close to the dispersing plate 8; the surface of each compression column 10 is fixedly connected with a compression head 11; the compression head 11 is semicircular in shape; the compression head 11 and the arc-shaped bulge 9 are arranged on the same axis; during operation, the conveying plate 6 drives the compression column 10 to move, the compression column 10 simultaneously drives the compression head 11 on the surface of the compression column to move, and in the moving process, the compression head 11 can be in contact with the arc-shaped protrusions 9 on the surface of the dispersion plate 8 and extrude, so that the dispersion plate 8 extrudes the extension spring 81 and rotates at a certain angle, and when the arc-shaped protrusions 9 and the compression head 11 are separated from each other, the dispersion plate 8 and the extension spring 81 are not extruded any more, so that the extension spring 81 and the dispersion plate 8 recover, and the dispersion plate 8 extrudes the ammonium persulfate bonded together, so that the ammonium persulfate is dispersed.
As shown in fig. 1 to 2, the number of the compression heads 11 on the surface of the single pressing column 10 is plural, and the compression heads are equidistantly arranged on the outer surface of the pressing column 10; the diameter of the compression head 11 is larger than that of the arc-shaped bulge 9; in operation, as the plurality of compression heads 11 are arranged, the compression heads 11 can intermittently contact and press the arc-shaped bulges 9, so that the dispersing plate 8 can intermittently rotate and recover, the dispersing speed of bonding ammonium persulfate is improved, and the drying of ammonium persulfate is facilitated.
Wherein, a telescopic rod 12 is fixedly connected with one side of the inner wall of the conveying pipeline 2, which is close to the dispersing plate 8; the outer surface of the telescopic rod 12 is fixedly connected with a limit spring 13; one end of the telescopic rod 12, which is close to the dispersing plate 8, is fixedly connected with a scraping head 14; when the dispersing plate 8 rotates under pressure, the dispersing plate 8 moves to one side close to the scraping head 14, and then contacts and extrudes the scraping head 14, so that the scraping head 14 drives the telescopic rod 12 to move, and the scraping head 14 can scrape ammonium persulfate adhered to the surface of the dispersing plate 8, thereby ensuring normal separation of the dispersing plate 8 on the ammonium persulfate.
As shown in fig. 5 to 6, a drying fan 15 is fixedly connected to the inside of the dryer 1; a cam shaft 16 is rotatably connected to the inside of the dryer 1; the inside of the dryer 1 is rotatably connected with a bearing plate 17; the bearing plate 17 is arranged near one side of the cam shaft 16; the lower surface of the receiving plate 17 and the inner wall of the dryer 1 are fixedly connected with an extrusion spring 18; it should be noted that, the camshaft 16 is connected to the output end of the external motor, and the connection mode is the prior art, and redundant description is omitted in this embodiment; when ammonium persulfate enters the surface of the bearing plate 17 in the dryer 1 through the conveying pipeline 2, hot air is blown into the dryer 1 by controlling the drying fan 15 to dry the ammonium persulfate, and meanwhile, the external motor drives the cam shaft 16 to rotate, the cam shaft 16 contacts with the lower surface of the bearing plate 17 and extrudes the cam shaft 16 when rotating, so that the bearing plate 17 rotates at a certain angle, the bearing plate 17 is inclined, when the cam shaft 16 and the bearing plate 17 are separated from each other, the bearing plate 17 returns under the action of the extrusion spring 18, so that the ammonium persulfate on the surface of the bearing plate 17 continuously rolls at a certain angle, and in the continuous rolling process, the hot air blown by the fan can dry different surfaces of the ammonium persulfate, so that the contact area of the ammonium persulfate and the hot air is improved, and the problem that the part of dark surface of the ammonium persulfate is difficult to dry in the prior art is solved.
An elastic post rod 19 is connected inside the bearing plate 17 in a sliding manner; the upper end of the elastic post rod 19 is fixedly connected with a pressing block 20; a compression bag 21 is fixedly connected to one side, close to the elastic post 19, of the inner part of the receiving plate 17; the outer surface of the compression bag 21 is fixedly connected with an air outlet pipe 22; when the ammonium persulfate is driven to rotate by the bearing plate 17, the ammonium persulfate can simultaneously give a certain pressure to the pressing block 20 in the bearing plate 17, so that the pressing block 20 drives the elastic post rod 19 to move, the elastic post rod 19 can squeeze the compression bag 21, gas in the compression bag 21 is squeezed out, and the gas is blown into the ammonium persulfate through the gas outlet pipe 22, so that the gas is completely contacted with the ammonium persulfate, and the drying efficiency of the ammonium persulfate is improved; the material of the compression bag 21 is rubber, and can be restored to the original state when the compression bag is not stressed.
The inside of the air outlet pipe 22 is fixedly connected with a one-way valve 23; the air outlet pipe 22 is obliquely arranged, and a one-way valve 23 is arranged, so that the air can be blown in one direction.
The inner wall of the dryer 1 is fixedly connected with a hot air pipeline 24; the hot air pipeline 24 is annularly arranged on the inner wall of the dryer 1; one end of the hot air pipeline 24 is connected with the output end of the drying fan 15; the annular hot air pipeline 24 can better enable hot air to be blown to the surface of the ammonium persulfate, and is convenient for drying the ammonium persulfate.
Further, the embodiment of the present invention will be described in detail with reference to specific embodiment 1 and embodiment 2:
example 1
The preparation method comprises the following steps of: 42% of ammonium persulfate and the balance of ammonium sulfate, and 5500L of mixed liquor of ammonium persulfate and ammonium sulfate is prepared, wherein the concentration of ammonium sulfate ions is 0.38g/mL, the concentration of ammonium sulfate ions is 1.1g/mL, the pH value is regulated to be 6.0 by adopting ammonia gas, the mixed liquor is introduced into a crystallization tank, when the temperature of the mixed liquor is maintained at 30 ℃, ammonium persulfate finished products with the particle size of 35 meshes are added as seed crystals, the temperature is slowly raised to 0.6 ℃ firstly, and then the temperature is reduced to-4 ℃ at the cooling rate of 9 ℃/h for cooling crystallization, so as to obtain a crystallization mixture; and then the crystallization mixture is introduced into the dryer 1, and the crystallization mixture is dried by each mechanism in the dryer 1 to obtain the ammonium persulfate crystal finished product.
The ammonium persulfate crystal grain size obtained in this example was 510. Mu.m.
Example 2
The preparation method comprises the following steps of: 50% of ammonium persulfate and the balance of ammonium sulfate, and 6000L of mixed liquor of ammonium persulfate and ammonium sulfate is prepared, wherein the concentration of ammonium sulfate ions is 0.36g/mL, the concentration of ammonium sulfate ions is 1.13g/mL, the pH value is regulated to 7.0 by adopting ammonia gas, the mixed liquor is introduced into a crystallization tank, when the temperature of the mixed liquor is maintained at 30 ℃, ammonium persulfate finished products with the particle size of 35 meshes are added as seed crystals, the temperature is slowly raised to 0.6 ℃ firstly, and then the temperature is reduced to-4 ℃ at the cooling rate of 8 ℃/h, so as to obtain a crystallization mixture; and then the crystallization mixture is introduced into the dryer 1, and the crystallization mixture is dried by each mechanism in the dryer 1 to obtain the ammonium persulfate crystal finished product.
The ammonium persulfate crystal grain size obtained in this example was 530. Mu.m.
When the wet solid ammonium persulfate is introduced into the conveying pipeline 2 through the feeding pipeline, the driving motor drives the rotating wheel 3 and the first connecting rod 4 to rotate, the first connecting rod 4 drives the second connecting rod 5 to rotate, the second connecting rod 5 can transversely and circularly reciprocate to drive the conveying plate 6 under the action of the first connecting rod 4 and the second connecting rod 5, the conveying plate 6 can continuously convey the wet solid ammonium persulfate into the dryer 1, meanwhile, the conveying plate 6 can be mutually contacted with the dispersing plate 8 in the moving process of the conveying pipeline 2, and certain pressure is given to the dispersing plate 8, so that the dispersing plate 8 is in a certain-amplitude open state, the dispersing plate 8 separates the ammonium persulfate bonded together, the problem that the ammonium persulfate is easy to bond together due to high ammonium persulfate humidity in the prior art is solved, and subsequent drying is facilitated; in the process that the conveying plate 6 drives the compression column 10 to move, the compression column 10 simultaneously drives the compression head 11 on the surface of the compression column to move, in the moving process, the compression head 11 is contacted with the arc-shaped protrusions 9 on the surface of the dispersion plate 8 and is extruded, so that the dispersion plate 8 extrudes the extension spring 81 and rotates at a certain angle, when the arc-shaped protrusions 9 are separated from the compression head 11, the dispersion plate 8 and the extension spring 81 are not extruded any more, and the extension spring 81 and the dispersion plate 8 recover, so that the dispersion plate 8 extrudes the ammonium persulfate bonded together, and therefore the ammonium persulfate is dispersed; because the plurality of compression heads 11 are arranged, the compression heads 11 can intermittently contact and press the arc-shaped bulges 9, so that the dispersing plate 8 can intermittently rotate and recover, the dispersing speed of bonding ammonium persulfate is improved, and the drying of the ammonium persulfate is facilitated; when the dispersing plate 8 rotates under pressure, the dispersing plate 8 moves to one side close to the scraping head 14, and then contacts and extrudes the scraping head 14, so that the scraping head 14 drives the telescopic rod 12 to move, and the scraping head 14 can scrape the ammonium persulfate adhered on the surface of the dispersing plate 8, thereby ensuring the normal separation of the dispersing plate 8 on the ammonium persulfate.
When ammonium persulfate enters the surface of the bearing plate 17 in the dryer 1 through the conveying pipeline 2, hot air is blown into the dryer 1 by controlling the drying fan 15 to dry the ammonium persulfate, and meanwhile, the external motor drives the cam shaft 16 to rotate, the cam shaft 16 contacts with the lower surface of the bearing plate 17 and extrudes the lower surface when rotating, so that the bearing plate 17 rotates at a certain angle, the bearing plate 17 is inclined, when the cam shaft 16 and the bearing plate 17 are separated from each other, the bearing plate 17 returns under the action of the extrusion spring 18, so that the ammonium persulfate on the surface of the bearing plate 17 continuously rolls at a certain angle, and in the continuous rolling process, the hot air blown by the fan can dry different surfaces of the ammonium persulfate, so that the contact area of the ammonium persulfate and the hot air is improved, and the problem that the dark surface of the ammonium persulfate is difficult to dry in the prior art is solved; when the receiving plate 17 drives the ammonium persulfate to rotate, the ammonium persulfate can simultaneously give a certain pressure to the pressing block 20 in the receiving plate 17, so that the pressing block 20 drives the elastic post rod 19 to move, the elastic post rod 19 can squeeze the compression bag 21, gas in the compression bag 21 is squeezed out, and the gas is blown into the ammonium persulfate through the gas outlet pipe 22, so that the gas is completely contacted with the ammonium persulfate, and the drying efficiency of the ammonium persulfate is improved; the material of the compression bag 21 is rubber, and the compression bag can be restored to an initial state when the compression bag is not stressed; the annular hot air pipeline 24 can better enable hot air to be blown to the surface of the ammonium persulfate, and is convenient for drying the ammonium persulfate.
In the description of the present invention, it should be understood that the terms "center," "longitudinal," "lateral," "front," "rear," "left," "right," "vertical," "horizontal," "top," "bottom," "inner," "outer," and the like indicate orientations or positional relationships based on the orientation or positional relationships shown in the drawings, merely to facilitate describing the present invention and simplify the description, and do not indicate or imply that the devices or elements referred to must have a specific orientation, be configured and operated in a specific orientation, and therefore should not be construed as limiting the scope of the present invention.
It should also be noted that unless explicitly stated or limited otherwise, the terms "disposed," "mounted," "connected," and "connected" are to be construed broadly, and may be, for example, fixedly connected, detachably connected, or integrally connected; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present invention can be understood by those of ordinary skill in the art according to the specific circumstances.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (6)
1. A preparation method of ammonium persulfate crystals is characterized by comprising the following steps of: the method comprises the following steps:
s1, proportioning: firstly, introducing ammonium persulfate into a batching box, adding ammonium sulfate in the batching process, stirring while adding the ammonium sulfate, wherein the stirring speed is 30-40r/min, so that the ammonium sulfate and the ammonium persulfate are fully dissolved to obtain a mixed material liquid of the ammonium persulfate and the ammonium sulfate, then introducing ammonia gas to enable the pH value to be 5.0-7.0, wherein the concentration of ammonium persulfate ions in the mixed material liquid is 0.35-0.45g/mL, and the ion concentration of the ammonium sulfate is 0.62-1.2g/mL;
s2, crystallizing: introducing ammonium persulfate and ammonium sulfate mixed feed liquid into a crystallization tank, controlling the temperature of the mixed feed liquid to be maintained at 28-35 ℃, adding ammonium persulfate finished products with the particle size of 30-40 meshes as seed crystals, slowly heating to 0.6-0.8 ℃, and then cooling to-4-6 ℃ at a cooling rate of 8-10 ℃/h for crystallization to obtain a crystallization mixture;
s3, drying: filtering the obtained crystallization mixture to obtain a solid, and introducing the obtained wet solid into a dryer (1) for drying to obtain ammonium persulfate crystal finished products;
in the step S2, calculated by the weight parts of the ammonium persulfate and ammonium sulfate mixed feed liquid, if the weight parts of the ammonium persulfate and ammonium sulfate mixed feed liquid are 8-12 parts, the adding amount of ammonium persulfate seed crystals is 18-22 parts;
the outer surface of the dryer (1) is fixedly connected with a conveying pipeline (2); the outer surface of the conveying pipeline (2) is rotatably connected with a rotating wheel (3); the rotating wheel (3) is connected with the output end of an external motor; the outer surface of the rotating wheel (3) is fixedly connected with a first connecting rod (4); the surface of the first connecting rod (4) is rotationally connected with a second connecting rod (5); one end of the second connecting rod (5) far away from the first connecting rod (4) is rotatably connected with a conveying plate (6); the width of the conveying plate (6) is matched with the width of the conveying pipeline (2); a plurality of turntables (7) are rotatably connected in the conveying pipeline (2); the outer surface of each turntable (7) is provided with a plurality of dispersing plates (8); a feeding pipeline is fixedly connected inside the conveying pipeline (2);
the outer surface of the dispersion plate (8) is fixedly connected with an arc-shaped bulge (9); the outer surface of the dispersion plate (8) is fixedly connected with an extension spring (81); one side of the conveying plate (6) close to the dispersing plate (8) is fixedly connected with symmetrically arranged pressing columns (10); the surface of each compression column (10) is fixedly connected with a compression head (11); the compression head (11) is semicircular in shape; the compression head (11) and the arc-shaped bulge (9) are arranged on the same axis;
the number of the single compression heads (11) on the surface of the compression column (10) is multiple, and the compression heads are equidistantly arranged on the outer surface of the compression column (10); the diameter of the compression head (11) is larger than that of the arc-shaped bulge (9).
2. The method for preparing ammonium persulfate crystal according to claim 1, wherein: a telescopic rod (12) is fixedly connected to one side, close to the dispersing plate (8), of the inner wall of the conveying pipeline (2); the outer surface of the telescopic rod (12) is fixedly connected with a limit spring (13); one end of the telescopic rod (12) close to the dispersing plate (8) is fixedly connected with a scraping head (14).
3. The method for preparing ammonium persulfate crystal according to claim 1, wherein: a drying fan (15) is fixedly connected inside the dryer (1); a cam shaft (16) is rotatably connected in the dryer (1); the inside of the dryer (1) is rotatably connected with a bearing plate (17); the bearing plate (17) is arranged close to one side of the cam shaft (16); the lower surface of the bearing plate (17) and the inner wall of the dryer (1) are fixedly connected with an extrusion spring (18); the camshaft (16) is connected to the output of the external motor.
4. The method for preparing ammonium persulfate crystal according to claim 3, wherein: an elastic post rod (19) is connected inside the bearing plate (17) in a sliding way; the upper end of the elastic post rod (19) is fixedly connected with a pressing block (20); a compression bag (21) is fixedly connected to one side, close to the elastic post rod (19), of the inner part of the bearing plate (17); the outer surface of the compression bag (21) is fixedly connected with an air outlet pipe (22).
5. The method for preparing ammonium persulfate crystal according to claim 4, wherein: a one-way valve (23) is fixedly connected inside the air outlet pipe (22); the air outlet pipe (22) is obliquely arranged.
6. The method for preparing ammonium persulfate crystal according to claim 5, wherein: the inner wall of the dryer (1) is fixedly connected with a hot air pipeline (24); the hot air pipeline (24) is annularly arranged on the inner wall of the dryer (1); one end of the hot air pipeline (24) is connected with the output end of the drying fan (15).
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665498A (en) * | 2019-02-14 | 2019-04-23 | 河北中科同创科技发展有限公司 | A kind of preparation method of ammonium persulfate crystalline solid |
| CN111998654A (en) * | 2020-08-24 | 2020-11-27 | 广州优讯环保科技有限公司 | Chemical fertilizer drying-machine |
| CN112678779A (en) * | 2021-02-02 | 2021-04-20 | 天津大学 | Preparation method of ammonium persulfate crystal |
| CN213514914U (en) * | 2020-07-02 | 2021-06-22 | 天津市鑫浩达化工有限公司 | Drying equipment for ammonium persulfate wet material |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109665498A (en) * | 2019-02-14 | 2019-04-23 | 河北中科同创科技发展有限公司 | A kind of preparation method of ammonium persulfate crystalline solid |
| CN213514914U (en) * | 2020-07-02 | 2021-06-22 | 天津市鑫浩达化工有限公司 | Drying equipment for ammonium persulfate wet material |
| CN111998654A (en) * | 2020-08-24 | 2020-11-27 | 广州优讯环保科技有限公司 | Chemical fertilizer drying-machine |
| CN112678779A (en) * | 2021-02-02 | 2021-04-20 | 天津大学 | Preparation method of ammonium persulfate crystal |
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