CN214485767U

CN214485767U - Novel lifting and fixing equipment with controllable particle size

Info

Publication number: CN214485767U
Application number: CN202023245918.2U
Authority: CN
Inventors: 颜志梁; 王隆肇; 游高平; 张刚; 彭贝利; 晁锋刚
Original assignee: Fujian Changqing New Energy Technology Co ltd
Current assignee: Fujian Changqing New Energy Technology Co ltd
Priority date: 2020-12-29
Filing date: 2020-12-29
Publication date: 2021-10-26
Anticipated expiration: 2030-12-29

Abstract

The utility model provides a controllable novel solid equipment of carrying of particle size, include: the device comprises a lifting and fixing device (23), a lifting and fixing pipeline (21) and a clear discharging pipeline (24) which are connected to the upper part of the lifting and fixing device (23), a lifting and fixing valve (22) arranged on the lifting and fixing pipeline, an observation port (232) connected to the top of the lifting and fixing device (23), a clear discharging valve (25) and an observation window (28) which are arranged on the clear discharging pipeline (24), a return pipeline (26) connected to the bottom of the lifting and fixing device (23), and a return valve (27) arranged on the return pipeline (26); and a plurality of layers of grid plates (234) which are stacked are transversely arranged in the lifting and fixing device (23). The utility model discloses a carry solid ware inside set up a plurality of be used for gathering the ternary precursor and quick grid board that deposits, can effectual change get into carry the overflow route of solid ware thick liquid and carrying the inside dwell time of solid ware, make the material deposit fast, finally improve thick liquids solid content and make the final product particle diameter controllable.

Description

Novel lifting and fixing equipment with controllable particle size

Technical Field

The utility model relates to a controllable novel solid equipment of carrying of particle diameter especially is used for improving the controllable novel solid equipment of carrying of particle diameter of ternary precursor thick liquids solid content.

Background

Lithium ion secondary batteries having high safety and high capacity have been widely noticed and used due to the environmental problems and the remarkable problem of energy consumption. The preparation method of the lithium ion cathode material precursor is also perfected.

In the preparation process of the nickel-cobalt-manganese ternary hydroxide, methods for improving the solid content of the slurry are various, wherein a thickener is an important mode for preparing the nickel-cobalt-manganese ternary hydroxide with narrow particle size distribution. At present, the method using the thickener has high cost, complex equipment operation, high equipment maintenance expense and low fault-tolerant rate.

SUMMERY OF THE UTILITY MODEL

The utility model provides a controllable novel solid equipment of carrying of grain diameter can effectively solve above-mentioned problem.

The utility model discloses a realize like this:

a novel consolidation apparatus of controllable particle size comprising: the device comprises a lifting and fixing device, a lifting and fixing pipeline, a lifting and fixing valve, a clear discharging pipeline, an observation port, a clear discharging valve and an observation window, a return pipeline and a return valve, wherein the lifting and fixing device is used for accumulating and quickly precipitating ternary precursors together; the interior of the lifting and fixing device is transversely provided with a plurality of layers of grid plates which are arranged in a stacked mode and used for accumulating and rapidly precipitating the ternary precursor; the clear pipeline of arranging further including set up in carry the connecting bend in the solid ware and set up in the filter screen in the connecting bend, just the import of connecting bend is towards carry the bottom of solid ware.

The utility model has the advantages that: the utility model discloses a carry the inside grid board that sets up a plurality of ternary precursors and gather and deposit fast of solid ware, through the rationalization design of height, inclination and the number of piles isoparametric of grid, can effectual change get into the overflow route of carrying solid ware thick liquid and carrying the inside dwell time of solid ware, reach the material and carrying the inside purpose of depositing fast of solid ware, finally improve thick liquids solid content, and then make it obtain good sphericity and make its particle diameter controllable.

Drawings

In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings that are required to be used in the embodiments will be briefly described below, it should be understood that the following drawings only illustrate some embodiments of the present invention, and therefore should not be considered as limiting the scope, and for those skilled in the art, other related drawings can be obtained according to the drawings without inventive efforts.

Fig. 1 is a schematic structural diagram of a novel reactor provided by an embodiment of the present invention.

Fig. 2 is a schematic structural diagram of a solid lifting unit in the novel reactor provided by the embodiment of the invention.

Fig. 3 is a top view of a grid plate in a lifting unit in the novel reactor provided by the embodiment of the present invention.

Fig. 4 is a flow chart of a method for preparing a ternary precursor by using the novel reactor according to an embodiment of the present invention.

FIG. 5 shows Ni prepared in example 1 of the present invention_0.5Co_0.2Mn_0.3(OH)₂Scanning electron micrographs of (A) and (B).

Detailed Description

To make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the drawings of the embodiments of the present invention are combined to clearly and completely describe the technical solutions of the embodiments of the present invention, and obviously, the described embodiments are 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. Thus, the following detailed description of the embodiments of the present invention, presented in the accompanying drawings, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. 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.

In the description of the present invention, the terms "first" and "second" are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically limited otherwise.

Referring to fig. 1, the present invention provides a novel reactor. The novel reactor is suitable for preparing ternary precursors.

The novel reactor comprises:

the reaction unit 10 comprises a reaction vessel 12, a feeding pipe 11 arranged in the reaction vessel 12, a stirring assembly arranged in the reaction vessel 12, a temperature control assembly 15 sleeved outside the bottom of the reaction vessel 12, an overflow pipeline 18 arranged on the upper part of the reaction vessel 12 and an overflow valve 17 arranged on the overflow pipeline 18;

the lifting and fixing unit 20 includes: the device comprises a lifting and fixing device 23 for accumulating and rapidly precipitating the ternary precursor, a lifting and fixing pipeline 21 respectively connected to the upper part of the lifting and fixing device 23 and the upper part of the reaction container 12, a lifting and fixing valve 22 arranged on the lifting and fixing pipeline 21, a drain pipeline 24 connected to the upper part of the lifting and fixing device 23, an observation port 232 connected to the top of the lifting and fixing device 23, a drain valve 25 and an observation window 28 arranged on the drain pipeline 24, a return pipeline 26 respectively connected to the bottom of the lifting and fixing device 23 and the bottom of the reaction container 12, and a return valve 27 arranged on the return pipeline 26. The supernatant valve 25 is used for discharging the supernatant liquid containing sulfur. The purge pipe 24 further includes a connection elbow 241 disposed in the extractor 23 and a filter screen 242 disposed in the connection elbow 241, and an inlet of the connection elbow 241 faces the bottom of the extractor 23.

The feed pipe 11 is used for introducing nickel-cobalt-manganese salt solution prepared according to a proportion. The reaction vessel 12, the stirring member and the temperature control member 15 may be of any conventional structure, and will not be described in detail herein. Further, the overflow pipe 18 is flush with the lifting and fixing pipe 21. The reaction unit 10 may further include an exit conduit 16.

Referring to fig. 2-3, the lifting device 23 is a top bucket, the bottom is an inverted cone, and the space volume is 1/3-1/2 of the effective volume of the reaction vessel 12. The material of the lifting and fixing device 23 is not limited, and can be any one of 316L steel and PP. Further, a plurality of layers of grid plates 234 which are arranged in a stacked manner and used for accumulating and rapidly precipitating the ternary precursor are transversely arranged in the lifting and fixing device 23; each grid plate 234 includes a plurality of grids 2342 arranged in an inclined manner, and the grids 2342 between two adjacent grid plates 234 are communicated with each other and the inclined directions of the grids 2342 are crossed. It can be understood that by arranging the grids 2342 obliquely and crossing the oblique directions, the solid can be accumulated and rapidly precipitated through continuous collision, and finally the overall morphology of the ternary precursor is improved. Preferably, the number of the grid plates 234 is 2-5 layers. It can be understood that when the number of grating plates 234 is small, the number of collisions is low and accumulation is difficult, and rapid sedimentation and morphology lifting are achieved; when the number is large, the particle size tends to be excessively large. Further, the angle formed by the axis of each grid 2342 and the lifter 23 is controlled to allow solids to accumulate and rapidly settle through continuous collision. Too small an angle results in too small a collision area, and too large an angle tends to accumulate in grating plate 234. Therefore, preferably, the axis of each grid 2342 forms an angle of 15 ° to 80 ° with the anchor 23. More preferably, the axis of each grid 2342 forms an angle of 25 ° to 35 ° with the anchor 23. In one embodiment, the axis of each grid 2342 forms an angle of about 30 ° with the lifting device 23.

Each grid plate 234 is 10-30 cm in height, and the distance from the top grid plate 234 to the top of the lifter 23 is 30-50 cm. The shape of each grid 2342 is not limited and can be selected according to actual needs; the shape of each grid 2342 may be a regular or irregular structure. In one embodiment, each grid 2342 is a regular hexagonal structure with sides of 5-20 centimeters.

As a further improvement, the backflow pipeline 26 includes two first bending discharging sections, a second bending discharging section connected to the first bending discharging section, a first extending section extending along the extending direction of the first bending discharging section, and a second extending section extending along the second bending discharging section in the opposite direction, and the first extending section and the second extending section are respectively provided with a first spiral push rod 262 and a second spiral push rod 264. The screw ejector pin can play a role in dredging when the backflow pipeline 26 is blocked.

The aperture of the filter screen 242 is 0.5um-15um, and in one embodiment, the aperture of the filter screen 242 is 9 um. The connecting bend 241 is directed towards the bottom of the carrier 23 so as to avoid clogging of the screen with particles.

Referring to fig. 4, an embodiment of the present invention further provides a method for preparing a ternary material precursor based on the novel reactor, including the following steps:

s1, adding a Ni/Co/Mn salt solution, an alkali solution and ammonia water into the reaction container 12 through a metering pump on a feeding pipe 11 according to the proportion, and simultaneously introducing inert gas for reaction, wherein the flow rate of the Ni/Co/Mn salt solution is 300L/h, the flow rate of the alkali solution is 96L/h, the flow rate of the ammonia water is 15L/h, and the Ni/Co/Mn ratio is 50.5%: 19.8%: 29.7% by mole;

s2, after reacting for 0.8-1.5 hours, fully opening the overflow valve 17, the lifting valve 22 and the backflow valve 27, and opening the purge valve 24 by 10-25%, wherein the excessive reaction liquid flow loss caused by the excessive opening of the purge valve 24 is not beneficial to discharging excessive clear liquid when the excessive reaction liquid flow loss is too small;

s3, controlling the reflux valve 27 to be opened or closed periodically to control the solid content volume ratio to reach a preset range, reducing the ammonia water concentration to 6-7g/L, and actually measuring the pH value to 11.2-11.4 to finally obtain an intermediate product with controllable particle size;

and S4, finally, carrying out post-treatment on the intermediate product to obtain the ternary material precursor.

Example 1:

adding Ni, Co and Mn into a mixture according to the weight percentage of 50.5%: 19.8%: 29.7 percent of nickel-cobalt-manganese salt solution prepared according to the molar ratio, 28 percent of alkali solution with mass concentration and 20 percent of ammonia water with mass concentration are added into the reaction container 12 through a metering pump, and 1m of feed liquid is introduced when the feed liquid is injected³The/h nitrogen gas, salt solution flow is 300L/h, and the alkali lye flow is 96L/h, and the aqueous ammonia flow is 15L/h, opens the alkaline metering pump of ammonia in proper order and injects into the reaction feed liquid and begin to react toward 12 insides of reaction vessel, begins to react 1 hour after, opens totally overflow valve 17 promote solid valve 22 and return valve 27, and will clear valve 24 opens 15%, return valve 27 opens 5 hours after, establishes return valve 27's closure duration is forAnd (3) 11h, wherein the opening time is 2h, the material color is observed, the solid content volume ratio is kept at about 9-10%, the ammonia water concentration is reduced to 6-7g/L, and the actual pH value is measured to 11.2-11.4, so that the intermediate product is finally obtained. Finally, the intermediate product is stirred and aged for 3 hours by the frequency of 10-20 Hz; removing the mother liquor by a centrifugal machine; adding the solid with the mother liquor removed into a sodium hydroxide solution with the concentration of 0.8mol/L and the temperature of 60 ℃, and circularly stirring for 15-60 minutes to obtain slurry; washing the slurry until the content of sodium element is less than or equal to 150ppm, and then drying and dehydrating; finally, the mixture is mixed to remove magnetism and is sieved by a 300-mesh sieve to finally obtain Ni with the particle size D50 of about 5um_0.5Co_0.2Mn_0.3(OH)₂。

Example 2:

the same as example 1 except that: after the reflux valve 27 is opened for 21 hours, the closing time of the reflux valve 27 is set to be 1.5 hours, the opening time is set to be 3 hours, and the solid content volume is kept at about 19-20% by observing the color of the material. Finally obtaining Ni with the grain diameter D50 of about 10um_0.5Co_0.2Mn_0.3(OH)₂。

The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims

1. A controllable novel solid equipment of carrying of grain size, its characterized in that includes: the device comprises a lifting and fixing device (23), a lifting and fixing pipeline (21) and a clear discharging pipeline (24) which are connected to the upper part of the lifting and fixing device (23), a lifting and fixing valve (22) arranged on the lifting and fixing pipeline, an observation port (232) connected to the top of the lifting and fixing device (23), a clear discharging valve (25) and an observation window (28) which are arranged on the clear discharging pipeline (24), a return pipeline (26) connected to the bottom of the lifting and fixing device (23), and a return valve (27) arranged on the return pipeline (26); wherein, a plurality of layers of grid plates (234) which are arranged in a stacked manner and used for accumulating and rapidly precipitating the ternary precursor are transversely arranged in the lifting and fixing device (23); the clear water discharging pipeline (24) further comprises a connecting bent pipe (241) arranged in the lifting device (23) and a filter screen (242) arranged in the connecting bent pipe (241), and an inlet of the connecting bent pipe (241) faces to the bottom of the lifting device (23).

2. The novel solid-lifting equipment with controllable particle size according to claim 1, characterized in that the bottom of the solid-lifting device (23) is in an inverted cone shape; and each grid plate (234) comprises a plurality of obliquely arranged grids (2342), and the grids (2342) between two adjacent layers of grid plates (234) are communicated with each other.

3. Novel lifting and fixing equipment with controllable particle size as claimed in claim 2, wherein the number of the grid plates (234) is 2-5 layers.

4. Novel lifting equipment with controllable particle size as claimed in claim 2, characterized in that the height of each grid plate (234) is 10-30 cm and the distance of the top grid plate (234) from the top of the lifting equipment (23) is 30-50 cm.

5. Novel lifting equipment with controllable particle size according to claim 2, characterized in that the axis of each grid (2342) forms an angle of 15-80 ° with the lifting equipment (23).

6. The novel lifting and fixing device with controllable particle size according to claim 2, wherein the backflow pipeline (26) comprises two first bending discharging sections, a second bending discharging section connected with the first bending discharging sections, a first extending section extending along the extending direction of the first bending discharging sections, and a second extending section extending along the opposite direction of the second bending discharging sections, and a first spiral ejector rod (262) and a second spiral ejector rod (264) are respectively arranged in the first extending section and the second extending section.

7. Novel lifting equipment with controllable particle size as claimed in claim 2, characterized in that the oblique directions of the grids (2342) between two adjacent layers of grid plates (234) are crossed.

8. The particle size controllable novel solid lifting device as claimed in claim 1, wherein the aperture of the filter screen (242) is 0.5um-15 um.