CN-119656929-B - High-shear dynamic mixing reaction device for preparing flexible particles and dynamic treatment process

CN119656929BCN 119656929 BCN119656929 BCN 119656929BCN-119656929-B

Abstract

The invention discloses a high-shear dynamic mixing reaction device for preparing flexible particles and a dynamic treatment process, which relate to the technical field of battery raw material preparation, wherein the process adopts a pulsation stress dynamic processing method to prepare flexible particle materials for batteries in a compact space on the basis of the existing chemical formula, the performances obtained by the material formula and the performance obtained by the pulsation stress dynamic processing complement each other to form an organic whole, the reaction device comprises a cylinder, the feed inlet has been seted up at the barrel top, and the discharge gate has been seted up to the barrel bottom, through rub the setting of turning over mixing mechanism to the rotation of (mixing) shaft is as the drive power of slider, makes the slider reciprocal slip in fixed sleeve, provides upwards and decurrent pressure for the material in the barrel, cooperates the setting of triangle fin on the baffle, and its pointed end can provide better shearing force for the moderately rotatory material granule, and the material is rubbed constantly and is stood up, tends to circularly, can make the carbon cladding more even.

Inventors

QUE ZHIJIAN
WANG MING
XIANG SHENGCHANG
CAO ZHENGXIANG
Que Muwang
MA JIJUAN
QUE YUAN

Assignees

浙江嘉吉石化工程有限公司
浙江长兴纽恩吉科技有限公司

Dates

Publication Date: 20260508
Application Date: 20250108

Claims (6)

1. The utility model provides a high shear dynamic mixing reaction device of preparation flexible granule, includes barrel (1), feed inlet (2) have been seted up at barrel (1) top, discharge gate (3) have been seted up to barrel (1) bottom, barrel (1) bottom outer wall fixedly connected with presss from both sides cover (4), the inner wall fixedly connected with spiral guide plate (5) of pressing from both sides cover (4), one side fixedly connected with in the outer wall of barrel (1) of pressing from both sides cover (4) is kept away from to spiral guide plate (5), its characterized in that still including: The kneading and turning mixing mechanism (6) is used for providing up-and-down reciprocating pressure and high shearing stirring for the materials in the cylinder (1); the self-adaptive gas distribution mechanism (7) is used for automatically regulating and controlling the gas distribution range to adapt to the mixing of different types of flexible particles by the device; The kneading and turning mixing mechanism (6) comprises a stirring shaft (67) which is rotationally connected to the top of the barrel (1), the bottom end of the stirring shaft (67) extends to the bottom of the barrel (1), a motor is fixedly connected to the top of the barrel (1), the top of the stirring shaft (67) penetrates through the top of the barrel (1) and is fixedly connected to the output end of the motor, a pair of raised strips (610) are fixedly connected to the middle of the stirring shaft (67), a stirrer (64) is slidingly connected with the outer walls of the stirring shaft (67) and the raised strips (610), a telescopic sleeve (63) is fixedly connected to the top of the stirrer, and the inner wall of the telescopic sleeve (63) is sleeved on the outer wall of the stirring shaft (67) in a sliding manner; The kneading and turning mixing mechanism (6) further comprises a pair of sliding blocks (69) fixedly connected to the top of the telescopic sleeve (63), the outer wall of the telescopic sleeve (63) is sleeved with a fixed sleeve (62) in a sliding manner, the inner wall of the fixed sleeve (62) is provided with a reciprocating thread groove (68), the outer walls of the sliding blocks (69) are connected in the reciprocating thread groove (68) in a sliding manner, the top of the fixed sleeve (62) is fixedly connected with a supporting frame (61), the top of the supporting frame (61) is fixedly connected to the inner wall of the top of the barrel (1), a plurality of baffle plates (65) are fixedly connected to the inner wall of the barrel (1) at equal intervals, and a plurality of triangular fins (66) are fixedly connected to two sides of each baffle plate (65); The self-adaptive gas distribution mechanism (7) comprises a rotary table (76) fixedly connected to the bottom of the stirring shaft (67), a plurality of limiting sleeves (75) are fixedly connected to the outer wall of the rotary table (76) at equal intervals, sliding rods (77) are slidably connected to the inner walls of the limiting sleeves (75), rotary blades (71) are fixedly connected to one sides, far away from the rotary table (76), of the sliding rods (77), springs (78) are fixedly connected to one sides, close to the rotary table (76), of the sliding rods (77), and one sides, far away from the sliding rods (77), of the springs (78) are fixedly connected to the inner walls of the rotary table (76); The self-adaptive gas distribution mechanism (7) further comprises a gas distributor (73) fixedly connected to the inner wall of the bottom of the cylinder body (1), a plurality of exhaust ports (74) are formed in the top and the bottom of the gas distributor (73), a gas inlet pipe (72) is fixedly communicated with the top of the gas distributor (73), and one side, far away from the gas distributor (73), of the gas inlet pipe (72) is fixedly penetrated through the outer walls of the cylinder body (1) and the jacket (4).
2. The high shear dynamic mixing reaction device for preparing flexible particles according to claim 1, wherein the gas distributor (73) has a flower shape, the top gas outlets (74) are uniformly distributed on the upper surface of the gas distributor (73), and the bottom gas outlets (74) are centrally distributed on the middle lower surface of the gas distributor (73).
3. The high shear dynamic mixing reaction device for preparing flexible particles according to claim 1, wherein the length of the stationary sleeve (62) is set to one third of the height of the cylinder (1).
4. The high shear dynamic mixing reaction device for preparing flexible particles according to claim 1, wherein the triangular fins (66) are staggered from each other on both sides of the baffle plate (65).
5. The high shear dynamic mixing reaction device for preparing flexible particles according to claim 1, wherein a heat transfer medium inlet is formed at the bottom of the jacket (4), and a heat transfer medium outlet is formed at the top of the jacket (4).
6. A high shear dynamic treatment process for preparing flexible particles, said process being carried out using a high shear dynamic mixing reaction device for preparing flexible particles according to any of claims 1-5, characterized in that said process comprises the steps of: The high shear mixing strengthening process comprises the steps that a rotating device consists of two stationary rings and two movable rings in a staggered sleeving manner, wherein a plurality of small holes are formed in the stationary rings, a cutter is arranged on the surface of each movable ring, materials enter an inner cavity of the rotating device from the center, flow out radially through the small holes in the first stationary ring under the centrifugal action of the rotating device, flow out radially through the small holes in the second stationary ring, and flow out radially through the small holes in the first stationary ring in a narrow channel formed between the two stationary rings by rotating an external movable ring, so that the materials which enter the second stationary ring radially form vertical shearing, and the materials which are mainly sheared at high speed are crushed and torn, so that the bottleneck of 500nm of particle diameter can be broken through, but the processed particle morphology is in an irregular form; on the basis of the original static temperature change synthesis principle, under the temperature change condition, the dynamic synthesis and sintering with the combined action of rheological stress and rheological shear stress and acceleration of thermochemical reaction and material mixing are added, and the materials are subjected to pressure, shear force and friction force in the cylinder (1) through a dynamic mixing reaction device and are continuously rubbed and turned over; 1. The rheological link is that chemical reaction synthesis is carried out in a barrel (1) with a stirring function, the reaction process is efficient piston reaction, the volume flow of a treated material in a unit reaction space is not more than 0.3 cubic meter in a unit reaction time, and the mixing times of the materials are more than 100 times, so that the consistency of the materials after the synthesis reaction is greatly improved; 2. Superplastic step, namely under the dynamic action of pulsation stress at proper temperature, particles are deformed due to grain boundary sliding accompanied with diffusion and dislocation, when the strain rate reaches a proper degree, the material has fine grain superplastic phenomenon, the crystal size is smaller than 15 mu m, the deformation temperature is higher, the strain rate epsilon is smaller than 0.3/S at 160 ℃ and above, and the stress on the material is larger than 3Mpa; 3. Although the dynamic sintering can supplement some synthetic reactions, the sintering function of lattice shaping is provided at the same time, for the high-temperature solid-state sintering, the sintering time is saved, the material burning-through is facilitated, and the energy consumption is reduced; 4. The carbon coating step is to adopt a pulsating stress dynamic stirring method, and the naphthenic aromatic hydrocarbon and the polar aromatic hydrocarbon can be rapidly removed under the action of shearing stress generated by stirring; The viscosity is reduced by stirring at the same temperature, the viscosity reduction is favorable for the formation of mesophase globules, and a good basis is provided for the development of the coated carbon in an ordered direction; Secondly, more intermediate phases are generated through stirring in a proper temperature range, because in the formed coated carbon, the more intermediate phases are contained in the generation process, the higher the order degree of the coated carbon formed by post-sintering is, the higher the graphitization degree is; Condition three, more and better mesophases are generated by time and agitation over the appropriate temperature range.

Description

High-shear dynamic mixing reaction device for preparing flexible particles and dynamic treatment process Technical Field The invention relates to the technical field of battery raw material preparation, in particular to a high-shear dynamic mixing reaction device for preparing flexible particles and a dynamic treatment process. Background The traditional high-temperature solid phase method generally mainly adopts a chemical formula to manufacture electrode materials, and because the materials to be processed are in a static state in the preparation process and are heated under the carrying of movable equipment, the change of mechanical parameters (such as elastic modulus E and the like) of the materials to be processed in the preparation process is not obvious, and meanwhile, the coated carbon is formed through the corresponding relationship between time and viscosity in the static state, and the materials in the static state in the preparation process do not have the condition of mutual mixing, so that the consistency of products is relatively poor after synthesis; In the working state process of the battery material, lithium ions carry electrons to shuttle in the material in the transmission process, the lithium ions flow into the material to expand, the lithium ions flow out of the material to shrink, and the expansion and shrinkage of the material cause flow stress, wherein the stress is diffusion stress, and the diffusion stress forms fatigue stress in a cyclic and reciprocating way along with the inflow and outflow of the lithium ions, and the fatigue stress is a main factor of damage and failure of battery particles; In order to obtain better conductivity, the coated carbon is required to be orderly formed, and the graphitization degree is as high as possible, but in the subsequent sintering process, the sintering temperature is determined by the electrical property of the battery material, generally, the temperature is about 700 ℃, and the sintering temperature required by needle coke (the orderly degree and the graphitization degree are obviously higher than those of common coke) at about 1450 ℃ is difficult to reach, so the graphitization degree is inevitably reduced; In the prior art, firstly, a sand mill with higher energy consumption is used, the raw materials are crushed into nano particles through the impact force of grinding balls for a plurality of hours, the particle diameter (d 50) can generally reach about 500 nanometers, if the particle diameter (d 50) is continuously lower than 500 nanometers, the energy consumption can be increased by times, the morphology of the material cannot be guaranteed to be spherical, secondly, the material is conveyed by dynamic equipment and is synthesized in a static mode through proper temperature and a plurality of hours, the process mainly comprises chemical reaction, the order and mechanical property of the coated carbon of the material are slightly improved, finally, the material is sintered at high temperature and subjected to lattice shaping in a static mode for a plurality of hours, and in the heating process, although the purpose of sintering and lattice shaping is achieved, the heat transfer of the material occupies a large amount of time, so that unnecessary energy consumption is caused; in addition, the existing dynamic mixing reactor has stronger pertinence, and is easy to generate excessive stirring for some reactions sensitive to stirring intensity in the preparation process of the battery nano raw materials, thereby causing the problems of side reaction or product quality reduction, thus generally requiring an additional mixing device and increasing equipment cost. Accordingly, the present invention provides a high shear dynamic mixing reaction apparatus and a dynamic processing technique for preparing flexible particles to overcome and ameliorate the shortcomings of the prior art. Disclosure of Invention In order to solve the technical problems, the invention provides a high-shear dynamic mixing reaction device and a dynamic treatment process for preparing flexible particles, which are used for solving the problems that in the prior art, the service life of a battery is shortened, the order degree of coated carbon is low, the consistency of prepared products is low (uniformity is insufficient) and the applicability of the device is low due to the fact that the diffusion stress of lithium ions in a material shuttles is large. In order to achieve the above purpose, the technical scheme adopted by the invention is that the high-shear dynamic mixing reaction device for preparing flexible particles and the dynamic treatment process comprise a cylinder, wherein the top of the cylinder is provided with a feed inlet, the bottom of the cylinder is provided with a discharge outlet, the outer wall of the bottom of the cylinder is fixedly connected with a jacket, the inner wall of the jacket is fixedly connected with a spiral guide plate, and one side