CN218530922U - Continuous pyrolysis device for preparing ultrapure lithium carbonate - Google Patents
Continuous pyrolysis device for preparing ultrapure lithium carbonate Download PDFInfo
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- CN218530922U CN218530922U CN202222884932.XU CN202222884932U CN218530922U CN 218530922 U CN218530922 U CN 218530922U CN 202222884932 U CN202222884932 U CN 202222884932U CN 218530922 U CN218530922 U CN 218530922U
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Abstract
The utility model discloses a continuous pyrolysis device for preparing ultrapure lithium carbonate belongs to lithium carbonate production field, has solved the problem that purity that present ultrapure lithium carbonate production technology exists is low, the granularity is inhomogeneous unstable, production efficiency is low. The utility model discloses a high-order storage groove and a plurality of pyrolysis cauldron, high-order storageThe preparation tank and each pyrolysis kettle are sequentially communicated through pipelines from top to bottom, each pipeline is provided with a control valve, the bottom of the lowermost pyrolysis kettle is provided with a liquid outlet valve, and the liquid outlet valve is connected with a centrifugal machine. Utilize the utility model discloses produce ultrapure lithium carbonate, liquid in each pyrolysis cauldron lasts limit business turn over in the production process, has realized the serialization production of lithium carbonate in the real meaning, has greatly shortened reaction cycle, has improved production efficiency. The Li content in the pyrolysis kettles can be kept in gradient, the reduction degree of the Li concentration is the same, and the Li content in the pyrolysis kettles can be kept in gradient 2 CO 3 The precipitation rate and the crystal growth rate are the same, and the purity and the granularity of the obtained ultrapure lithium carbonate are stable and uniform.
Description
Technical Field
The utility model belongs to lithium carbonate production field, concretely relates to continuous pyrolysis device for preparing ultrapure lithium carbonate.
Background
With the progress of the times and the development of science and technology, li2CO3 is widely applied to the fields of ceramics, glass, atomic energy, aerospace, lithium batteries, lithium alloys, medicines and the like, and is also a raw material for preparing various lithium compounds. Due to different applications, different requirements are imposed on the purity and particle size of lithium carbonate. 99.9 percent of high-purity lithium carbonate is used as a positive electrode material of the lithium ion battery; 99.99% of high-purity lithium carbonate is used as an electrolyte of the lithium ion battery; 99.999% of ultrapure lithium carbonate is used in medicine and surface elastic wave element materials. With the continuous expansion of the application range of lithium products in the high-tech field, the demand for lithium salts is increasing at home and abroad, the requirements on the purity of the products are higher and higher, and the requirements on the particle size are also harsher, so that the development of high-added-value ultra-pure lithium salt products with different particle sizes is imperative.
SUMMERY OF THE UTILITY MODEL
The utility model aims at providing a continuous pyrolysis device for preparing ultrapure lithium carbonate to solve the problem that the purity that present ultrapure lithium carbonate production technology exists is low, the granularity is inhomogeneous unstable, production efficiency is low.
The technical scheme of the utility model is that: the utility model provides a continuous pyrolysis device for preparing ultrapure lithium carbonate, includes high-order storage groove and a plurality of pyrolysis cauldron, and high-order storage groove and each pyrolysis cauldron communicate in proper order through the pipeline from top to bottom, are equipped with control flap on each pipeline, and the pyrolysis cauldron bottom of lower floor is equipped with out the liquid valve, and centrifuge is connected to the play liquid valve.
As the utility model discloses a further improvement is equipped with agitating unit in the pyrolysis cauldron to guarantee that the heating is even, the lithium carbonate crystallization is even.
As a further improvement, the pyrolysis kettle is communicated with a steam pipe, the pyrolysis kettle adopts a steam heating mode, and the heating efficiency is high.
As a further improvement of the utility model, the outer wall of the pyrolysis kettle is provided with a heat preservation layer.
As a further improvement of the utility model, the bottom of the pyrolysis kettle is conical. Aiming at the characteristic that the lithium carbonate is easy to scar, the conical design can weaken the scar of the lithium carbonate, and is more beneficial to continuous production.
As a further improvement, the utility model is provided with a flowmeter on each pipeline, which is convenient for monitoring and adjusting the flow.
As a further improvement of the utility model, the control valve and the liquid outlet valve are all electromagnetic valves.
Putting the lithium bicarbonate solution into a high-level storage tank; opening each control valve from top to bottom in sequence to enable the lithium bicarbonate solution to flow downwards automatically and flow into each pyrolysis kettle in sequence, closing each control valve, heating the pyrolysis kettles, starting pyrolysis reaction in each pyrolysis kettle, controlling the reaction, enabling the Li content of liquid in each pyrolysis kettle to gradually decrease from top to bottom to form a gradient, then opening each control valve from top to bottom in sequence to enable the liquid in each reaction kettle to enter liquid and exit liquid while performing pyrolysis reaction, enabling the liquid in the lowest pyrolysis kettle to exit liquid to a centrifugal machine for centrifugation, monitoring the Li content of the liquid in each pyrolysis kettle in the continuous reaction process, controlling the opening degree of each control valve and the heating degree of each pyrolysis kettle to enable the Li content in each pyrolysis kettle to keep the gradient, enabling the lithium bicarbonate solution in each pyrolysis kettle to continuously enter and exit and keep the pyrolysis reaction, and continuously performing pyrolysis to produce lithium carbonate.
The beneficial effects of the utility model are that: utilize the utility model discloses produce ultrapure lithium carbonateAnd the liquid in each pyrolysis kettle continuously enters and exits at the same time in the production process, so that the continuous production of the lithium carbonate is realized in the real sense, the reaction period is greatly shortened, and the production efficiency is improved. The Li content in a plurality of pyrolysis kettles can be kept in gradient, and the reduction degree of the Li concentration is the same, so the Li in unit time 2 CO 3 The precipitation rate is the same, the crystal growth rate is also the same, the precipitation of the ultrapure lithium carbonate is reduced according to a concentration gradient mode, the purity and the granularity of the obtained ultrapure lithium carbonate are stable and uniform, and the purity and the granularity of the obtained ultrapure lithium carbonate both meet the industrial standard. The utility model discloses simple structure, easy to carry out has fine spreading value.
Drawings
Fig. 1 is a schematic structural diagram of a first embodiment of the present invention.
In the figure: 1-a pyrolysis kettle; 2-a pipeline; 3-controlling the valve; 4-high reserve tank; 5-a centrifuge; 6-steam pipe; 7-a stirring device; 8-an insulating layer; 9-a liquid outlet valve; 10-flow meter.
Detailed Description
The present invention will be described in detail with reference to the accompanying drawings.
Examples 1,
As shown in fig. 1, a continuous pyrolysis device for preparing ultrapure lithium carbonate comprises a high-order storage tank 4 and a plurality of pyrolysis kettles 1, wherein the high-order storage tank 4 and each pyrolysis kettle 1 are sequentially communicated through a pipeline 2 from top to bottom, each pipeline 2 is provided with a control valve 3, the bottom of the pyrolysis kettle 1 at the lowermost layer is provided with a liquid outlet valve 9, and the liquid outlet valve 9 is connected with a centrifuge 5.
A stirring device 7 is arranged in the pyrolysis kettle 1. A steam pipe 6 is communicated in the pyrolysis kettle 1. The outer wall of the pyrolysis kettle 1 is provided with a heat preservation layer 8. The bottom of the pyrolysis kettle 1 is conical.
Each pipe 2 is provided with a flow meter 10.
The control valve 3 and the liquid outlet valve 9 are both electromagnetic valves.
In this embodiment, the number of the pyrolysis reactors 1 is 3. Control valves 3 are arranged between the high-position storage tank 4 and the first pyrolysis kettle 1 (the uppermost layer), between the first pyrolysis kettle 1 and the second pyrolysis kettle 1, and between the second pyrolysis kettle 1 and the third pyrolysis kettle 1 (the lowermost layer), and liquid outlet valves 9 are arranged between the third pyrolysis kettle 1 and the centrifuge 5.
The using method comprises the following steps:
A. and (3) placing the purified lithium bicarbonate solution into a high-level storage tank 4, wherein the content of Li in the lithium bicarbonate solution is 8g/L.
B. B, placing the lithium bicarbonate solution obtained in the step A into a high-level storage tank 4; sequentially opening each control valve 3 from top to bottom to enable the lithium bicarbonate solution to flow downwards and flow into each pyrolysis kettle 1 in sequence, wherein the liquid level in each pyrolysis kettle 1 is about two thirds of the kettle body, closing each control valve 3, introducing high-temperature steam into each pyrolysis kettle 1 through a steam pipe 6, starting pyrolysis reaction in each pyrolysis kettle 1, and controlling the reaction to enable the Li content of the liquid in the first pyrolysis kettle 1 (the uppermost layer) to reach 6g/L, the Li content of the liquid in the second pyrolysis kettle 1 to reach 4g/L, and the Li content of the liquid in the third pyrolysis kettle 3 (the lowermost layer) to reach 2g/L; then, the control valves 3 and the liquid outlet valve 9 are opened from top to bottom in sequence, so that the liquid in each pyrolysis kettle 1 is fed while the pyrolysis reaction is performed, and the liquid is discharged from the liquid outlet valve 9 to the centrifuge 5 for centrifugation, wherein the liquid in the third pyrolysis kettle 3 is discharged from the centrifuge. Lithium bicarbonate solution is continuously from high-order reserve tank 4 to first pyrolysis cauldron 1, from first pyrolysis cauldron 1 to second pyrolysis cauldron 1, from second pyrolysis cauldron 1 to third pyrolysis cauldron 1, from third pyrolysis cauldron 1 to centrifuge 5, go into while going out continuous pyrolysis and carry out serialization production, the Li content of liquid in each pyrolysis cauldron 1 is monitored in the reaction process that lasts, through the degree of opening of controlling each control flap 3 and play liquid valve 9 and the heating degree of each pyrolysis cauldron 1, the Li content in each pyrolysis cauldron 1 keeps above-mentioned gradient.
C. And washing the wet lithium carbonate centrifuged by the centrifuge 5 with water, and then calcining and drying to obtain qualified ultrapure lithium carbonate.
Purity test results: 99.99915%. And (3) granularity test results: d10:1.7 μm, D50:6 μm, D90:14 μm.
This example 5 set was repeated and the experimental data are shown in table 1.
As can be seen from the table 1, the prepared ultrapure lithium carbonate has stable purity and granularity by carrying out continuous pyrolysis in a mode of carrying out gradient reduction of 2g/L while carrying out feeding and discharging, not only meets the industry YS/T582-2013 standard, but also has small purity and granularity fluctuation and is very stable.
Examples 2,
In this embodiment, the number of the pyrolysis reactors 1 is 2. All be equipped with control valve 3 between high-order reserve tank 4 and first pyrolysis cauldron 1 (the superiors), between first pyrolysis cauldron 1 and second pyrolysis cauldron 1 (the bottommost layer), be equipped with out liquid valve 9 between second pyrolysis cauldron 1 and the centrifuge 5.
The method of use is similar to that of example 1, and during the reaction, the Li content of the liquid in the first pyrolysis reactor 1 is kept at 5g/L and the Li content of the liquid in the second pyrolysis reactor 1 is kept at 2g/L.
Purity test results: 99.9986 percent. The result of the particle size test is as follows: d10:4 μm, D50:13 μm, D90:21 μm.
Examples 3,
In this embodiment, the number of the pyrolysis reactors 1 is 6. Control valves 3 are arranged between the high-level reserve tank 4 and the first pyrolysis kettle 1 (the uppermost layer) and between the adjacent pyrolysis kettles 1, and liquid outlet valves 9 are arranged between the sixth pyrolysis kettle 1 (the lowermost layer) and the centrifugal machine 5.
Similar to the example 1, during the reaction, the Li content of the liquid in the first pyrolysis kettle 1 is kept at 7g/L, the Li content of the liquid in the second pyrolysis kettle 1 is kept at 6g/L, the Li content of the liquid in the third pyrolysis kettle 1 is kept at 5g/L, the Li content of the liquid in the fourth pyrolysis kettle 1 is kept at 4g/L, the Li content of the liquid in the fifth pyrolysis kettle 1 is kept at 3g/L, and the Li content of the liquid in the sixth pyrolysis kettle 1 is kept at 2g/L.
Purity test results: 99.99911%. The result of the particle size test is as follows: d10:2 μm, D50:4.4 μm, D90:11.5 μm.
As can be seen from comparison of examples 1-3, during continuous step pyrolysis, the Li content in the solution is reduced according to 3g/L, the purity of the prepared lithium carbonate is less than 99.999%, and the particle size index does not meet the YS/T582-2013 standard. The Li content is reduced according to 1g/L and 2g/L, the purity of the prepared lithium carbonate is over 99.999 percent, and the granularity also meets the YS/T582-2013 standard, the two modes can be used for producing the ultra-pure lithium carbonate, but the process route for preparing the ultra-pure lithium carbonate according to 1g/L reduction is longer, a plurality of pyrolysis kettles are used, the requirement on the height of a workshop is met when the lithium carbonate is used for self-flowing, and the preparation of the ultra-pure lithium carbonate according to 2g/L reduction is comprehensively considered to be better.
Claims (7)
1. A continuous pyrolysis device for preparing ultrapure lithium carbonate is characterized in that: including high-order reserve groove (4) and a plurality of pyrolysis cauldron (1), high-order reserve groove (4) and each pyrolysis cauldron (1) communicate in proper order through pipeline (2) from top to bottom, are equipped with control flap (3) on each pipeline (2), and pyrolysis cauldron (1) bottom of lower floor is equipped with liquid outlet valve (9), and centrifuge (5) are connected in liquid outlet valve (9).
2. A continuous pyrolysis apparatus for the preparation of ultrapure lithium carbonate according to claim 1, characterized in that: a stirring device (7) is arranged in the pyrolysis kettle (1).
3. A continuous pyrolysis apparatus for the preparation of ultrapure lithium carbonate according to claim 1 or 2, characterized in that: a steam pipe (6) is communicated in the pyrolysis kettle (1).
4. A continuous pyrolysis apparatus for the preparation of ultrapure lithium carbonate according to claim 3, characterized in that: and the outer wall of the pyrolysis kettle (1) is provided with a heat-insulating layer (8).
5. The continuous pyrolysis apparatus for preparing ultrapure lithium carbonate according to claim 4, characterized in that: the bottom of the pyrolysis kettle (1) is conical.
6. A continuous pyrolysis apparatus for the preparation of ultrapure lithium carbonate according to claim 5, characterized in that: each pipeline (2) is provided with a flowmeter (10).
7. The continuous pyrolysis apparatus for preparing ultrapure lithium carbonate according to claim 6, characterized in that: the control valve (3) and the liquid outlet valve (9) both adopt electromagnetic valves.
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| CN202222884932.XU CN218530922U (en) | 2022-11-01 | 2022-11-01 | Continuous pyrolysis device for preparing ultrapure lithium carbonate |
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| CN202222884932.XU CN218530922U (en) | 2022-11-01 | 2022-11-01 | Continuous pyrolysis device for preparing ultrapure lithium carbonate |
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