CN218307917U - Reaction kettle - Google Patents
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- CN218307917U CN218307917U CN202222104698.4U CN202222104698U CN218307917U CN 218307917 U CN218307917 U CN 218307917U CN 202222104698 U CN202222104698 U CN 202222104698U CN 218307917 U CN218307917 U CN 218307917U
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Abstract
The utility model discloses a reaction kettle, which is used for reasonably regulating and controlling stirring shearing force in the reaction process and comprises a reaction cavity, a first baffle group, a second baffle group and a stirring component; the stirring assembly comprises a stirring shaft, a first stirring paddle and a second stirring paddle, and the second stirring paddle is positioned between the first stirring paddle and the bottom wall of the reaction cavity; the first baffle plate group comprises a plurality of first baffle plates, each first baffle plate is arranged on the side wall of the reaction cavity through a first adjusting mechanism corresponding to the first baffle plate, the first adjusting mechanisms are used for driving the first baffle plates to rotate around a first axis, and the first axis is parallel to the axis of the stirring shaft; the second baffle group comprises a plurality of second baffles, each second baffle is arranged on the side wall of the reaction cavity through a second adjusting mechanism corresponding to the second baffle, the second adjusting mechanism is used for driving the second baffles to rotate around a second axis, and the second axis is parallel to the axis of the stirring shaft; the first stirring paddle is positioned between the first baffle group and the second baffle group.
Description
Technical Field
The utility model relates to a material preparation technical field, in particular to reation kettle.
Background
The nickel-cobalt-manganese ternary positive electrode material has the advantages of low price, stable performance and relatively balanced capacity and safety, so the nickel-cobalt-manganese ternary positive electrode material is widely applied to lithium ion batteries of digital products, power supplies and energy storage devices. The method is characterized in that a nickel-cobalt-manganese salt solution, an alkali solution and an ammonia solution are introduced into a reaction kettle, and a nickel-cobalt-manganese ternary material precursor is prepared by a coprecipitation method, wherein the main methods comprise a continuous method and an intermittent method. Due to the rapid development and trend of the electric automobile industry in recent years, expectations and requirements for energy density, safety, stability and specific charge-discharge capacity of lithium ion batteries are higher and higher. Because the particle size distribution and the material structure of the layered ternary material have great influence on the energy density and the stability of the battery, and the ternary material has inheritance to the structure and the particle size of the precursor, the preparation of the precursor with an ideal structure and particle size distribution becomes a problem which needs to be considered urgently at present.
SUMMERY OF THE UTILITY MODEL
The utility model discloses a reaction kettle for rationally regulate and control stirring shearing force in the reaction process.
In order to achieve the above purpose, the utility model provides the following technical scheme:
a reaction vessel comprising: the reaction chamber, and a first baffle group, a second baffle group and a stirring assembly which are positioned in the reaction chamber;
the stirring assembly comprises a stirring shaft, a first stirring paddle and a second stirring paddle, wherein the first stirring paddle and the second stirring paddle are arranged on the stirring shaft, and the second stirring paddle is positioned between the first stirring paddle and the bottom wall of the reaction cavity;
the first baffle group comprises a plurality of first baffles, each first baffle is arranged on the side wall of the reaction cavity through a corresponding first adjusting mechanism, the first adjusting mechanisms are used for driving the first baffles to rotate around a first axis, and the first axis is parallel to the axis of the stirring shaft;
the second baffle group comprises a plurality of second baffles, each second baffle is arranged on the side wall of the reaction cavity through a second adjusting mechanism corresponding to the second baffle, the second adjusting mechanisms are used for driving the second baffles to rotate around a second axis, and the second axis is parallel to the axis of the stirring shaft;
the arrangement direction of the first baffle group and the second baffle group is parallel to the axis of the stirring shaft, and the first stirring paddle is positioned between the first baffle group and the second baffle group along the axis direction of the stirring shaft.
Above-mentioned reation kettle adopts double-deck baffle design about the upper and lower double-deck baffle design first baffle group and second baffle group promptly, the stirring subassembly has double-deck stirring rake about having first stirring rake and second stirring rake, and the first stirring rake that is located the upper strata is located between first baffle group and the second baffle group, first baffle group includes a plurality of first baffles, the second baffle group includes a plurality of second baffles, and the first baffle that corresponds from top to bottom and second baffle are all rotatable, with the different region of adjustment reaction chamber (the first half region that corresponds with first baffle group and the latter half region that corresponds with second baffle group) shearing performance, specifically rotate in the same direction as or the stirring direction of contrary (mixing) shaft through the first baffle of first adjustment mechanism drive, rotate the realization in the same direction as or the stirring direction of contrary (mixing) shaft through the second adjustment mechanism drive second baffle. The embodiment of the utility model provides a reation kettle can adjust the distribution of coprecipitation method preparation precursor technology reation kettle internal shear force and torrent intensity along with time and space, the improvement of selectivity or reduction granule collision probability to prepare the precursor granule of high sphericity and qualified particle diameter.
In some embodiments, a first baffle in the first baffle group corresponds to a second baffle in the second baffle group one to one, and the arrangement directions of the first baffle and the second baffle which correspond to each other are parallel to the axis of the stirring shaft.
In some embodiments, the first baffle rotates about the first axis by an angle θ 1 In the range ofComprises the following steps: theta is more than or equal to 60 degrees 1 Less than or equal to 60 degrees; and/or the presence of a gas in the gas,
an angle θ of the second baffle rotating around the second axis 2 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 2 ≤60°。
In some embodiments, the first adjustment mechanism comprises: the device comprises a first hinge, a first driving rod and a first transmission assembly, wherein one end of the first hinge is connected with the first baffle, and the other end of the first hinge is connected with the inner wall of the reaction cavity; the axis of the first driving rod is parallel to the axis of the stirring shaft, and the first driving rod is in transmission connection with the first baffle plate through the first transmission assembly; and/or the presence of a gas in the gas,
the second adjustment mechanism includes: one end of the second hinge is connected with the second baffle, and the other end of the second hinge is connected with the inner wall of the reaction cavity; the axis of the second driving rod is parallel to the axis of the stirring shaft, and the second driving rod is in transmission connection with the second baffle through the second transmission assembly.
In some embodiments, the first transmission assembly is a gear pair; and/or the presence of a gas in the gas,
the second transmission assembly is a gear pair.
In some embodiments, the first adjusting mechanism further comprises a first guide assembly, the first guide assembly comprises a first guide rail and a first guide groove in sliding fit with the first guide rail, and the first guide groove is an arc-shaped groove; the first guide rail is arranged on the inner wall, and the first guide groove is arranged on the first baffle; and/or the first guide rail is arranged on the first baffle plate, and the first guide groove is arranged on the inner wall; and/or the presence of a gas in the gas,
the second adjusting mechanism further comprises a second guide assembly, the second guide assembly comprises a second guide rail and a second guide groove in sliding fit with the second guide rail, and the second guide groove is an arc-shaped groove; the second guide rail is arranged on the inner wall, and the second guide groove is arranged on the second baffle; and/or the second guide rail is arranged on the second baffle, and the second guide groove is arranged on the inner wall.
In some embodiments, in the first barrier and the second barrier which correspond to each other, the first driving rod and the second driving rod are the same driving rod, and the driving rod drives the first barrier and the second barrier to rotate in opposite directions simultaneously.
In some embodiments, the first baffle and the second baffle are rectangular plates and both extend in a direction parallel to the axis of the stirring shaft;
the width of the first baffle is larger than that of the second baffle; and/or the presence of a gas in the gas,
the length of the first baffle is less than the length of the second baffle.
In some embodiments, the length a of the first baffle 1 Comprises the following steps:
length a of the second baffle 2 Comprises the following steps:
wherein H is the height of the liquid level in the reaction cavity; and/or the presence of a gas in the gas,
width b of the first baffle 1 Comprises the following steps:
width b of the second baffle 2 Comprises the following steps:
wherein T is the diameter of the reaction chamber.
In some embodiments, the distance D between the first baffle group and the second baffle group along the direction parallel to the axis of the stirring shaft is:
wherein H is the height of the liquid level in the reaction cavity.
Drawings
Fig. 1 is a schematic structural diagram of a reaction kettle according to an embodiment of the present invention;
FIG. 2 is a schematic view of the first baffle and the second baffle rotated by a certain angle;
FIG. 3 is a schematic diagram of the arrangement of first baffles in the reaction kettle;
FIG. 4 is a schematic view of the transmission structure at A in FIG. 3;
FIG. 5 is a schematic view showing the arrangement of second baffles in the reaction vessel;
FIG. 6 is a schematic view of the transmission structure at B in FIG. 5;
FIG. 7 is a schematic view showing the rotation directions of the first baffle and the second baffle in the first working state of the reaction kettle;
FIG. 8 is a schematic view showing the rotation directions of the first baffle and the second baffle in the second working state of the reaction vessel;
fig. 9 is a schematic view of the rotation directions of the first baffle and the second baffle in the third working state of the reaction kettle.
Icon: 1-a reaction chamber; 2-a first baffle; 3-a second baffle; 4-a stirring component; 5-a first adjustment mechanism; 6-a second adjustment mechanism; 11-a first liquid inlet pipe; 12-a second liquid inlet pipe; 13-a third feed tube; 14-a discharge outlet; 15-overflow pipe; 16-a fixed groove; 41-stirring shaft; 42-a first paddle; 43-a second stirring paddle; 44-a stirring motor; 51-a first hinge; 52-a first drive rod; 53-a first transmission assembly; 54-a first guide assembly; 61-a second hinge; 62-a second drive rod; 63-a second transmission assembly; 64-a second guide assembly; 531-first gear teeth; 532-second gear teeth; 541-a first guide rail; 542-first guide groove; 631-third gear teeth; 632-transition gear; 633-fourth gear teeth; 641-a second guide rail; 642-second guide groove.
Detailed Description
In the production process of the precursor, the lack of stirring shearing force easily causes poor sphericity of the product, and precursor particles grow to a certain diameter in a reaction kettle and cannot bear the shearing force to be broken, namely, the phenomenon of spherical cracking causes the capacity of the prepared anode material to be attenuated, so that the electrochemical performance is reduced, the quality of the product is reduced, and the synthesis of the material is not facilitated. The conventional solution is to reduce the stirring speed during the reaction to reduce the shearing force with the reaction, but the reduction of the speed will reduce the dispersibility of the feed solution and is not favorable for the reaction. Therefore, the problem that stirring and shearing force are reasonably regulated and controlled in the reaction process so as to prepare the qualified ternary cathode material precursor is urgently needed to be solved.
The technical solutions in the embodiments of the present invention will be described clearly and completely with reference to the accompanying drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments in the present invention, all other embodiments obtained by a person skilled in the art without creative work belong to the protection scope of the present invention.
As shown in fig. 1, an embodiment of the present invention provides a reaction kettle, including: the reaction device comprises a reaction cavity 1, and a first baffle group, a second baffle group and a stirring assembly 4 which are positioned in the reaction cavity 1; the stirring assembly 4 comprises a stirring shaft 41, and a first stirring paddle 42 and a second stirring paddle 43 which are arranged on the stirring shaft 41, and the second stirring paddle 43 is positioned between the first stirring paddle 42 and the bottom wall of the reaction chamber 1; the first baffle plate group comprises a plurality of first baffle plates 2, each first baffle plate 2 is arranged on the side wall of the reaction chamber 1 through a first adjusting mechanism 5 corresponding to the first baffle plate 2, and the first adjusting mechanisms 5 are used for driving the first baffle plates 2 to rotate around a first axis which is parallel to the axis of the stirring shaft 41; the second baffle group comprises a plurality of second baffles 3, each second baffle 3 is arranged on the side wall of the reaction chamber 1 through a second adjusting mechanism 6 corresponding to the second baffle 3, the second adjusting mechanism 6 is used for driving the second baffles 3 to rotate around a second axis, and the second axis is parallel to the axis of the stirring shaft 41; the arrangement direction of the first baffle group and the second baffle group is parallel to the axis of the stirring shaft 41, and the first stirring paddle 42 is positioned between the first baffle group and the second baffle group along the axis direction of the stirring shaft 41.
Above-mentioned reation kettle adopts double-deck baffle design about the upper and lower double-deck baffle design promptly first baffle group and second baffle group, stirring subassembly 4 has about double-deck stirring rake promptly first stirring rake 42 and second stirring rake 43, and the first stirring rake 42 that is located the upper strata is located between first baffle group and the second baffle group, first baffle group includes a plurality of first baffles 2, the second baffle group includes a plurality of second baffles 3, and the first baffle 2 and the second baffle 3 that correspond from top to bottom are all rotatable, in order to adjust 1 different regions in reaction chamber (the first half region that corresponds with first baffle group and the latter half region that corresponds with the second baffle group) shear performance, specifically rotate in the same direction as or contrary (mixing) shaft 41's stirring direction through the first baffle 2 of first adjustment mechanism 5 drive, rotate through the stirring direction of second adjustment mechanism 6 drive second baffle 3 in the same direction as or contrary (mixing) shaft 41 and realize. The embodiment of the utility model provides a reation kettle can adjust the distribution of coprecipitation method preparation precursor technology reation kettle internal shear force and torrent intensity along with time and space, the improvement of selectivity or reduction granule collision probability to prepare the precursor granule of high sphericity and qualified particle diameter.
In a possible implementation manner, referring to fig. 1, a first liquid inlet pipe 11, a second liquid inlet pipe 12 and a third liquid inlet pipe 13 are further disposed on the reaction kettle, for example, the first liquid inlet pipe 11 is used for conveying alkali liquor to the reaction chamber 1, the second liquid inlet pipe 12 is used for conveying salt liquor to the reaction chamber 1, and the third liquid inlet pipe 13 is used for conveying ammonia liquor to the reaction chamber 1. The upper part of the reaction kettle is also provided with an overflow pipe 15, and the bottom of the reaction kettle is provided with a discharge port 14. The stirring assembly 4 comprises a stirring motor 44 and a stirring shaft 41 in transmission connection with the stirring motor 44, the stirring shaft 41 is connected with a first stirring paddle 42 and a second stirring paddle 43, and the first stirring paddle 42 is positioned at the upper part of the second stirring paddle 43; the first stirring paddle 42 is positioned between the first baffle group and the second baffle group, and the second stirring paddle 43 is not lower than the arc-shaped bottom of the reaction chamber 1, so that solid particles carried by the rotation of the fluid are prevented from being accumulated in the acute angle area between the lower second baffle group and the bottom wall to form a flowing 'dead zone'. The first set of baffles comprises 2-6 first baffles 2, for example the first set of baffles comprises 4 first baffles 2, the second set of baffles comprises 2-6 second baffles 3, for example the second set of baffles comprises 4 second baffles 3.
In some embodiments, the first baffle 2 in the first baffle group corresponds to the second baffle 3 in the second baffle group one by one, and the arrangement direction of the first baffle 2 and the second baffle 3 in one-to-one correspondence is parallel to the axis of the stirring shaft 41.
In a possible implementation manner, the first baffle 2 and the second baffle 3 correspond to each other one by one, and the first baffle 2 is located right above the second baffle 3.
In some embodiments, the first baffle 2 is rotated about the first axis by an angle θ 1 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 1 Less than or equal to 60 degrees; and/or the angle theta of rotation of the second shutter 3 about the second axis 2 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 2 ≤60°。
In a possible implementation manner, the first adjusting mechanism 5 drives the first baffle 2 to rotate around the first axis in a first direction, and the second adjusting mechanism 6 drives the second baffle 3 to rotate around the second axis in a second direction, where the first direction is opposite to the second direction, so as to realize the inclination of the upper and lower baffles in opposite directions, illustratively, the first direction is clockwise direction, and the second direction is counterclockwise direction, or the first direction is counterclockwise direction, and the second direction is clockwise direction. Referring to fig. 2, the first barrier 2 is rotated about a first axis by an angle θ 1 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 1 ≦ 60 °, e.g. θ 1 Is-60 °, -50 °, -40 °, -30 °, -20 °, -10 °, -5 °, 10 °, 20 °, 30 °, 40 °, 50 °, or 60 °; angle theta of rotation of the second shutter 3 about the second axis 2 The range of (A) is as follows: theta is more than or equal to 60 degrees 2 ≦ 60 °, e.g. θ 2 Is-60 °, -50 °, -40 °, -30 °, -20 °, -10 °, -5 °, 10 °, 20 °, 30 °, 40 °, 50 °, or 60 °. It should be noted that the sign of the angle only indicates the direction of rotation, i.e. clockwise or counterclockwise, for example-45 ° indicates a counterclockwise rotation of 45 ° and 45 ° indicates a clockwise rotation of 45 °.
In some embodiments, the first adjustment mechanism 5 comprises: a first hinge 51, a first driving rod 52 and a first transmission assembly 53, wherein one end of the first hinge 51 is connected with the first baffle 2, and the other end is connected with the inner wall of the reaction chamber 1; the axis of the first driving rod 52 is parallel to the axis of the stirring shaft 41, and the first driving rod 52 is in transmission connection with the first baffle 2 through a first transmission assembly 53; and/or the second adjusting mechanism 6 comprises: a second hinge 61, a second driving rod 62 and a second transmission assembly 63, wherein one end of the second hinge 61 is connected with the second baffle 3, and the other end is connected with the inner wall of the reaction chamber 1; the axis of the second driving rod 62 is parallel to the axis of the stirring shaft 41, and the second driving rod 62 is in transmission connection with the second baffle 3 through a second transmission assembly 63.
In a possible implementation manner, referring to fig. 3 and 4, the inner wall of the reaction chamber 1 is provided with a fixing groove 16 opened toward the stirring shaft 41, and the first baffle plate 2 is positioned in the fixing groove 16. The first adjustment mechanism 5 includes: first hinge 51, first actuating lever 52 and first drive assembly 53, first baffle 2 is connected with the internal wall face of reaction chamber 1 through first hinge 51, and first actuating lever 52 is located fixed slot 16, and stirring shaft 41 one side is kept away from to first baffle 2 is connected with the transmission of first drive assembly 53, and first actuating lever 52 is connected with the transmission of first drive assembly 53 for drive first baffle 2 rotates around the first axis, and is exemplary, and the first axis is the axis of first actuating lever 52.
In a possible mode of realization, referring to fig. 5 and 6, the inner wall of the reaction chamber 1 is provided with a fixing groove 16 opened toward the stirring shaft 41, and the second baffle 3 is located in the fixing groove 16. The second adjustment mechanism 6 includes: second hinge 61, second actuating lever 62 and second transmission assembly 63, second baffle 3 passes through second hinge 61 and is connected with the internal wall face of reaction chamber 1, second actuating lever 62 is located fixed slot 16, second baffle 3 keeps away from (mixing) shaft 41 one side and is connected with second transmission assembly 63 transmission, second actuating lever 62 is connected with second transmission assembly 63 transmission for drive second baffle 3 rotates around the second axis, and is the axis of second actuating lever 62 for the example, first axis.
In some embodiments, first drive assembly 53 is a gear pair; and/or the second transmission assembly 63 is a gear pair.
In a possible way of realisation, with reference to fig. 4, the first transmission assembly 53 comprises a first gear tooth 531 and a second gear tooth 532 meshing with the first gear tooth 531, the first gear tooth 531 being arranged on the side of the first shutter 2 remote from the stirring axle 41, and the second gear tooth 532 being arranged on the side of the first driving lever 52 facing the first shutter 2. Illustratively, incomplete gears are arranged on the first baffle 2 and the first driving rod 52, so that the first baffle 2 can rotate around the axis of the first driving rod 52 and the rotation range can be met.
In a possible implementation manner, referring to fig. 6, the second transmission assembly 63 includes a third gear 631, a transition gear 632, and a fourth gear 633, the third gear 631 is disposed on a side of the second barrier 3 away from the stirring shaft 41, the fourth gear 633 is disposed on a side of the second driving rod 62 facing the second barrier 3, and the fourth gear 633 is in meshing transmission with the third gear 631 through the transition gear 632. Exemplarily, the second baffle 3 and the second driving rod 62 are both provided with incomplete gears, so that the second baffle 3 can rotate around the axis of the second driving rod 62 and can meet the rotation range.
In some embodiments, the first adjusting mechanism 5 further includes a first guiding assembly 54, the first guiding assembly 54 includes a first guiding rail 541 and a first guiding groove 542 slidably engaged with the first guiding rail 541, and the first guiding groove 542 is an arc-shaped groove; the first guide rail 541 is disposed on the inner wall, and the first guide groove 542 is disposed on the first baffle 2; and/or, the first guide rail 541 is disposed on the first baffle 2, and the first guide groove 542 is disposed on the inner wall; and/or the second adjusting mechanism 6 further includes a second guiding assembly 64, the second guiding assembly 64 includes a second guiding rail 641 and a second guiding groove 642 slidably engaged with the second guiding rail 641, and the second guiding groove 642 is an arc-shaped groove; the second guide rail 641 is disposed on the inner wall, and the second guide groove 642 is disposed on the second baffle 3; and/or, the second guide rail 641 is disposed on the second baffle 3, and the second guide groove 642 is disposed on the inner wall.
In a possible implementation manner, with continued reference to fig. 4, in order to ensure the stability of the rotation of the first baffle plate 2, a first guiding assembly 54 is disposed between the first baffle plate 2 and the inner wall of the reaction chamber 1, the first guiding assembly 54 includes a first guide rail 541 and a first guide groove 542 slidably engaged with the first guide rail 541, the first guide groove 542 is an arc-shaped groove, and the center of the arc-shaped groove is located on the axis of the first driving rod 52. The first guide rail 541 is installed on the first barrier 2 toward the second barrier 3, and the first guide groove 542 is disposed on both side walls of the fixing groove 16. The first guide rail 541 cooperates with the first guide groove 542 to restrain a rotation direction and seal.
In a possible implementation manner, with continued reference to fig. 6, in order to ensure the stability of the rotation of the second baffle plate 3, a second guiding assembly 64 is disposed between the second baffle plate 3 and the inner wall of the reaction chamber 1, the second guiding assembly 64 includes a second guiding rail 641 and a second guiding groove 642 slidably engaged with the second guiding rail 641, the second guiding groove 642 is an arc-shaped groove, and the center of the arc-shaped groove is located on the axis of the second driving rod 62. The second guide rail 641 is installed on one side of the second barrier 3 departing from the first barrier 2, and the second guide groove 642 is disposed on two side walls of the fixing groove 16. The second guide rail 641 and the second guide groove 642 cooperate to restrict the rotation direction and seal.
In some embodiments, in the first barrier 2 and the second barrier 3 corresponding to each other, the first driving rod 52 and the second driving rod 62 are the same driving rod, and the driving rods simultaneously drive the first barrier 2 and the second barrier 3 to rotate reversely.
In a possible way, with continued reference to fig. 1 in conjunction with fig. 4 and 6, the first driving rod 52 and the second driving rod 62 are the same driving rod, that is, the driving rod drives the first shutter 2 and the second shutter 3 to rotate in opposite directions. The driving rod can be rotated manually to adjust the rotating angles of the first baffle 2 and the second baffle 3, and the driving rod can also be controlled to rotate by a motor. Specifically, the second gear 532 on the driving rod directly engages with the first gear 531 on the first barrier 2, and the fourth gear 633 on the driving rod engages with the third gear 631 on the second barrier 3 through the transition gear 632, for example, when the driving rod rotates clockwise, the first barrier 2 rotates counterclockwise, and the second barrier 3 rotates clockwise.
The upper baffle plate and the lower baffle plate rotate in a staggered way by manually rotating the driving rod and are complementary with the included angle of the wall surface of the reaction cavity 1; the shearing force of the upper layer and the lower layer can be adjusted, so that the shearing force of the lower layer at the early stage is high, and the high-sphericity matrix particles are formed after the materials flow in; and the upper layer is in a low-shearing force state, so that the weakening of the cycle performance caused by the over-strong shearing force in the whole reaction kettle is avoided. Along with the reaction, the lower baffle is inclined (when the plane of the baffle passes through the axis of the stirring shaft 41, the baffle is in a non-inclined state), the inclined direction is consistent with the rotating direction, the shearing force of the lower layer is reduced, and the ball cracking in the later reaction period is avoided; the rotation directions of the upper baffle and the stirring paddle are opposite, the shearing effect is more obvious, but due to the structural characteristics of short and wide parts, the high-shearing area in the kettle occupies a small area, and the vortex can be effectively eliminated.
In some embodiments, the first baffle 2 and the second baffle 3 are both rectangular plates, and both extend in a direction parallel to the axis of the stirring shaft 41; the width of the first baffle 2 is larger than that of the second baffle 3; and/or the length of the first baffle 2 is less than the length of the second baffle 3.
In a possible way, with continued reference to fig. 1, the first baffle plate 2 and the second baffle plate 3 are rectangular plates and both extend in a direction parallel to the axis of the stirring shaft 41, where extending in a direction parallel to the axis of the stirring shaft 41 is understood to mean that the length of the first baffle plate 2 in a direction parallel to the axis of the stirring shaft 41 is greater than the length of the first baffle plate 2 in a direction perpendicular to the axis of the stirring shaft 41, and the length of the second baffle plate 3 in a direction parallel to the axis of the stirring shaft 41 is greater than the length of the second baffle plate 3 in a direction perpendicular to the axis of the stirring shaft 41. As shown in fig. 1, the width of the first barrier 2 is greater than the width of the second barrier 3, and the length of the first barrier 2 is less than the length of the second barrier 3. First baffle 2 is upper baffle broad promptly, can effectively eliminate the swirl that the center stirring caused.
In some embodiments, the length a of the first baffle 2 1 Comprises the following steps:
length a of the second shutter 3 2 Comprises the following steps:
wherein H is the height of the liquid level in the reaction cavity 1; and/or the width b of the first baffle 2 1 Comprises the following steps:
width b of the second shutter 3 2 Comprises the following steps:
wherein T is the diameter of the reaction chamber 1.
In a possible way of realisation, with continued reference to fig. 1, the length a of the first baffle 2 1 Is composed of
Or
Length a of the second shutter 3 2 Is composed of
Or
Width b of the first baffle 2 1 Is composed of
Or
Width b of the second shutter 3 2 Is composed of
Or
In some embodiments, the distance D between the first baffle group and the second baffle group in the direction parallel to the axis of the stirring shaft 41 is:
wherein H is the height of the liquid level in the reaction chamber 1.
In one possible implementation manner, with continued reference to fig. 1, the distance D between the first baffle group and the second baffle group is
Or
The utility model provides an among the mode that probably realizes, after letting in the material in the reation kettle at the initial stage of reaction, make first baffle group and second baffle group maintain the state of figure 7, the (mixing) shaft is along the stirring of clockwise, the second baffle is the reverse stirring direction of rotation slope of lower floor's baffle promptly, first baffle is upper baffle in the same direction as the direction of rotation slope promptly, from the fluid mechanics angle analysis, reation kettle the latter half regional shear behavior reinforcing this moment, saline and alkaline ammonia solution gets into behind the reation kettle under strong shear flow effect dispersion and nucleation, and strong shear force can improve precursor nucleation sphericity. Because the upper layer baffle is wider, the vertical plane projection at the inclination angle of the baffle is wider than that of the lower layer baffle, and the vortex generated near the liquid surface during stirring can be effectively eliminated. After the slurry becomes turbid and opaque gradually from clear and transparent and the D50 is increased to 3 mu m, the first baffle group and the second baffle group are kept in the state shown in the figure 8 and continuously operated. This time similar to the flow characteristics of a conventional reactor. The particle size gradually increased and the D50 increased to 8 μm, and then the first baffle group and the second baffle group were maintained in the state shown in fig. 9. The turbulence degree of the lower layer is weakened at the moment, and the collision probability of the particles is lowered so as to avoid the breaking of the spheres by the large particles. At the moment, the stirring rotating speed does not need to be reduced too much, thereby ensuring that the materials flow into the reaction kettle and then are quickly dispersed in the kettle. The upper baffle is wider, can form the torrent and hinder liquid level vortex formation, and the upper baffle is shorter, and is less to the turbulent kinetic energy and the torrent dissipation rate influence in most region in the cauldron. And the first stirring paddle, namely the rotational flow formed by stirring of the upper stirring paddle, is not hindered between the double-layer baffles, and the horizontal section of the rotational flow is superposed with the horizontal section of the reaction kettle.
Exemplarily, 1, preparing a nickel salt, a cobalt salt and a manganese salt into a solution A with the concentration of 0.8-4mol/L, preparing an alkali solution B with the concentration of 0.5-10mol/L, and preparing a complexing agent solution C with the concentration of 0.5-15 mol/L;
2. introducing the solutions A, B and C into a reaction kettle through a constant flow pump, introducing protective gas, and controlling the conditions such as flow, temperature, reaction pH value, stirring speed and the like to enable the first baffle group and the second baffle group to maintain the state shown in the figure 7;
3. after the D50 is increased to 3 microns, rotating a rotating wheel at the top of the reaction kettle, maintaining the first baffle group and the second baffle group in the state shown in the figure 8, continuously operating, and gradually increasing the particle size;
4. after the D50 is increased to 8 mu m, a rotating wheel at the top of the reaction kettle is rotated to maintain the first baffle group and the second baffle group in the state shown in the figure 9, at the moment, the turbulence degree of the lower layer is weakened, and the collision probability of the particles is reduced, so that the large particles are prevented from breaking the spheres. The angle of inclination of the baffle plate can be gradually increased as the particle size is increased.
The stirring rotating speed does not need to be excessively reduced in the whole process, so that the slurry in the middle and later stages of the reaction still has good dispersing performance when being in a high viscosity state, the solution in the later stage can be quickly dispersed after flowing into the reaction kettle, and micro powder precursor particles generated by local high concentration are avoided.
The following detailed description of the present invention is provided by using a specific embodiment, namely, the preparation of a high sphericity crack-free ternary precursor by adjusting the inclination angle of the baffle:
the specific operation method comprises the following steps:
(1) Nickel sulfate, cobalt sulfate and manganese sulfate are mixed according to the proportion of Ni: co: the molar ratio of Mn is 0:0.10:0.10, a mixed solution A of nickel, cobalt and manganese with the total concentration of 2.0mol/L, and NaOH aqueous solution B with the concentration of 8mol/L and ammonia aqueous solution C with the concentration of 10mol/L are prepared.
(2) Introducing deionized water, ammonia water and alkali solution into the reaction kettle, adjusting ammonia concentration to 10g/L and pH value to 11, starting stirring at 500rpm, maintaining temperature at 60 deg.C, introducing solution A at 60mL/min, maintaining ammonia concentration at 8-9g/L and pH value at 10.5-11.5, and adjusting the inclination angle theta as shown in FIG. 7 1 ＝45°。
(3) When the reaction product D is 50 to 3 mu m, adjusting a baffle theta of the reaction kettle 1 =30 °, while the stirring speed was reduced to 480rpm.
(4) When the reaction product D is 50 to 5 mu m, adjusting a baffle theta of the reaction kettle 1 =0 °, i.e. the state of fig. 8, while the stirring speed was reduced to 460rpm.
(5) Continuously reacting until the D50 is increased to 8 mu m, and adjusting a baffle theta of the reaction kettle 1 = 45 °, i.e. the state of fig. 9, while the stirring speed was adjusted to 450rpm.
(6) Sustained reaction to D50 increaseAdjusting the baffle theta of the reaction kettle to 11 mu m 1 = -60 °, i.e. the situation in fig. 9, while the stirring speed is adjusted to 430rpm.
(7) Stopping the machine, discharging, aging, washing and drying to obtain the required precursor particles.
It will be apparent to those skilled in the art that various changes and modifications may be made to the embodiments of the present invention without departing from the spirit and scope of the invention. Thus, if such modifications and variations of the present invention fall within the scope of the claims of the present invention and their equivalents, the present invention is also intended to include such modifications and variations.
Claims (10)
1. A reaction kettle, comprising: the reaction chamber, and a first baffle group, a second baffle group and a stirring assembly which are positioned in the reaction chamber;
the stirring assembly comprises a stirring shaft, a first stirring paddle and a second stirring paddle, wherein the first stirring paddle and the second stirring paddle are arranged on the stirring shaft, and the second stirring paddle is positioned between the first stirring paddle and the bottom wall of the reaction cavity;
the first baffle group comprises a plurality of first baffles, each first baffle is arranged on the side wall of the reaction cavity through a corresponding first adjusting mechanism, the first adjusting mechanisms are used for driving the first baffles to rotate around a first axis, and the first axis is parallel to the axis of the stirring shaft;
the second baffle group comprises a plurality of second baffles, each second baffle is arranged on the side wall of the reaction cavity through a second adjusting mechanism corresponding to the second baffle, the second adjusting mechanism is used for driving the second baffles to rotate around a second axis, and the second axis is parallel to the axis of the stirring shaft;
the arrangement direction of the first baffle group and the second baffle group is parallel to the axis of the stirring shaft, and the first stirring paddle is positioned between the first baffle group and the second baffle group along the axis direction of the stirring shaft.
2. The reaction kettle according to claim 1, wherein a first baffle in the first baffle group corresponds to a second baffle in the second baffle group one by one, and the arrangement directions of the first baffle and the second baffle which correspond to each other are parallel to the axis of the stirring shaft.
3. The reactor of claim 2, wherein the first baffle rotates about the first axis by an angle θ 1 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 1 Less than or equal to 60 degrees; and/or the presence of a gas in the gas,
an angle θ of rotation of the second baffle about the second axis 2 The range of (A) is as follows: theta is more than or equal to 60 degrees below zero 2 ≤60°。
4. The reactor of claim 1, wherein the first adjustment mechanism comprises: one end of the first hinge is connected with the first baffle, and the other end of the first hinge is connected with the inner wall of the reaction cavity; the axis of the first driving rod is parallel to the axis of the stirring shaft, and the first driving rod is in transmission connection with the first baffle plate through the first transmission assembly; and/or the presence of a gas in the gas,
the second adjustment mechanism includes: one end of the second hinge is connected with the second baffle, and the other end of the second hinge is connected with the inner wall of the reaction cavity; the axis of the second driving rod is parallel to the axis of the stirring shaft, and the second driving rod is in transmission connection with the second baffle through the second transmission assembly.
5. The reactor according to claim 4, wherein the first transmission assembly is a gear pair; and/or the presence of a gas in the gas,
the second transmission assembly is a gear pair.
6. The reaction kettle of claim 4, wherein the first adjusting mechanism further comprises a first guide assembly, the first guide assembly comprises a first guide rail and a first guide groove in sliding fit with the first guide rail, and the first guide groove is an arc-shaped groove; the first guide rail is arranged on the inner wall, and the first guide groove is arranged on the first baffle; and/or the first guide rail is arranged on the first baffle plate, and the first guide groove is arranged on the inner wall; and/or the presence of a gas in the atmosphere,
the second adjusting mechanism further comprises a second guide assembly, the second guide assembly comprises a second guide rail and a second guide groove in sliding fit with the second guide rail, and the second guide groove is an arc-shaped groove; the second guide rail is arranged on the inner wall, and the second guide groove is arranged on the second baffle; and/or the second guide rail is arranged on the second baffle plate, and the second guide groove is arranged on the inner wall.
7. The reaction kettle of claim 4, wherein the first baffle and the second baffle corresponding to each other are the same driving rod, and the driving rod drives the first baffle and the second baffle to rotate in opposite directions at the same time.
8. The reactor according to any one of claims 1 to 7, wherein the first baffle and the second baffle are rectangular plates and extend in a direction parallel to the axis of the stirring shaft;
the width of the first baffle is larger than that of the second baffle; and/or the presence of a gas in the atmosphere,
the length of the first baffle is less than the length of the second baffle.
9. The reactor of claim 8, wherein the length a of the first baffle is 1 Comprises the following steps:
length a of the second baffle 2 Comprises the following steps:
wherein H is the transThe liquid level in the reaction chamber; and/or the presence of a gas in the atmosphere,
width b of the first baffle 1 Comprises the following steps:
width b of the second baffle 2 Comprises the following steps:
wherein T is the diameter of the reaction chamber.
10. The reactor according to any one of claims 1 to 7, wherein a distance D between the first baffle group and the second baffle group in a direction parallel to the axis of the stirring shaft is:
wherein H is the height of the liquid level in the reaction cavity.
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| CN202222104698.4U CN218307917U (en) | 2022-08-10 | 2022-08-10 | Reaction kettle |
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| CN202222104698.4U CN218307917U (en) | 2022-08-10 | 2022-08-10 | Reaction kettle |
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