Crystallization equipment for producing lithium difluoro (oxalato) borate

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By designing a crystallization equipment for the production of lithium difluoroxalate, the gradient cooling technology is used to solve the problems of fine particle size and long drying time during the synthesis process, and the effect of efficient crystallization and rapid output is achieved.

CN222534138UActive Publication Date: 2025-02-28ROLECHEM (SHANDONG) CO LTD

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Patent Information

Application Number: CN202421278775.0
Authority / Receiving Office: CN · China
Patent Type: Utility models(China)
Current Assignee / Owner
Filing Date: 2024-06-05
Publication Date: 2025-02-28
Estimated Expiration: 2034-06-05

AI Technical Summary

Technical Problem

During the synthesis of lithium difluoroxalate borate, the particle size is relatively fine, resulting in the drying time of ordinary drying equipment that affects production capacity and product quality.

Method used

A crystallization equipment including a first-stage horizontal transistor, a film scraper and a second-stage horizontal transistor was designed. Gradient cooling is achieved through a first-stage cooling system and a second-stage cooling system, increasing the crystallinity of the product and improving crystallization efficiency.

Benefits of technology

It achieves efficient crystallization and rapid output of the product, reduces drying time, and improves production capacity and product quality.

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Abstract

The utility model discloses crystallization equipment for producing lithium difluoro (oxalato) borate, which comprises a first-stage horizontal crystallization pipe, a film scraper and a second-stage horizontal crystallization pipe, the first-stage horizontal crystallization pipe is connected with a first-stage cooling system, the second-stage horizontal crystallization pipe is connected with a second-stage cooling system, and materials are crystallized by the first-stage horizontal crystallization pipe and then are cooled by the second-stage cooling system. A feeding hole of the first-stage horizontal crystallization pipe is connected with a discharging hole of a first-stage material transfer pump through a pipeline, a feeding hole of the first-stage material transfer pump is connected with a discharging hole of a first-stage feeding bin through a pipeline, a feeding hole of the first-stage feeding bin is connected with a discharging hole of a first-stage feeding valve through a pipeline, and a discharging hole of a second-stage feeding valve is connected with a discharging hole of a second-stage feeding valve through a pipeline; a feeding port of the first-stage feeding valve is connected with an external pipeline, raw materials are crystallized through the first-stage horizontal crystallization pipe, the first-stage cooling system is started, then the raw materials are pumped into the second-stage horizontal crystallization pipe, the second-stage cooling system is started, gradient cooling is achieved, the crystallinity of products is increased, and efficient crystallization and rapid output of the products are achieved.

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Description

Technical Field

[0001] The utility model relates to the technical field of crystallization equipment, in particular to a crystallization equipment for producing lithium difluorooxalate borate. Background Art

[0002] As a lithium salt additive, lithium difluorooxalate borate is currently mainly used in power batteries. Lithium difluorooxalate borate can form an excellent SEI film on the surface of the negative electrode, improving the battery's cycle performance and high and low temperature performance. Lithium difluorooxalate borate can improve the safety of the battery. Lithium difluorooxalate borate can protect the battery aluminum foil and improve the battery cycle life. Lithium difluorooxalate borate can reduce the generation of hydrogen fluoride in electrolytes containing LiPF6. In addition, lithium difluorooxalate borate also has a series of advantages such as high conductivity, good thermal stability under normal working conditions, and a wide voltage window. As an electrolyte salt, it exhibits excellent performance in batteries and has excellent compatibility with lithium cobalt oxide, lithium iron phosphate, and positive electrode materials in ternary battery systems. As a lithium-ion battery electrolyte, lithium difluorooxalate borate has good thermal stability, electrochemical stability and good cyclability. When it is used in solid electrolytes, its stable anions will improve the structure and composition of the passivation layer between the electrolyte and the negative electrode material interface, which is beneficial to the stability of the electrolyte, passivation film, and electrode. When lithium difluorooxalatoborate is used in lithium batteries, there are relatively strict requirements on its solvent residues. For certain specific solvents, it is necessary to control it within 3000ppm or even lower.

[0003] However, due to the fine particle size during the synthesis process, ordinary drying equipment has a long drying time, which affects production capacity and product quality. Utility Model Content

[0004] In order to solve the above technical problems, the utility model provides a crystallization device for producing lithium difluorooxalate borate, comprising a primary horizontal crystallization tube, a scraper and a secondary horizontal crystallization tube, wherein the primary horizontal crystallization tube is connected to a primary cooling system, the secondary horizontal crystallization tube is connected to a secondary cooling system, the scraper is connected to a heating system, and after the material is crystallized in the primary horizontal crystallization tube, it enters the scraper for evaporation and concentration, and then is pumped into the secondary horizontal crystallization tube for crystallization.

[0005] Preferably: the feed port of the first-level horizontal crystallization tube is connected to the discharge port of the first-level transfer pump through a pipeline, the feed port of the first-level transfer pump is connected to the discharge port of the first-level feed bin through a pipeline, the feed port of the first-level feed bin is connected to the discharge port of the first-level feed valve through a pipeline, and the feed port of the first-level feed valve is connected to an external pipeline.

[0006] Preferably, the discharge port of the first-stage horizontal crystallization tube is connected to the feed port of the first-stage discharge valve through a pipeline, and the discharge port of the first-stage discharge valve is connected to the first-stage filter through a pipeline.

[0007] Preferably, one discharge port of the primary filter is connected to a primary filter cake silo, and another discharge port of the primary filter is connected to a feed port of a primary filtrate transfer tank.

[0008] Preferably, the discharge port of the primary filtrate transfer tank is connected to the feed port of the transfer transfer pump through a pipeline, and the discharge port of the transfer transfer pump is connected to the feed port of the scraper through a pipeline.

[0009] Preferably, a discharge port of the film scraper is connected to a feed port of a solvent condenser through a pipeline, and a discharge port of the solvent condenser is connected to a feed port of a solvent receiving tank through a pipeline.

[0010] Preferably, another outlet of the film scraper is connected to the feed inlet of the secondary feed bin through a pipeline.

[0011] Preferably, the discharge port of the secondary feed bin is connected to the feed port of the secondary feed transfer pump via a pipeline, and the discharge port of the secondary feed transfer pump is connected to the feed port of the secondary horizontal crystallization tube via a pipeline.

[0012] Preferably: the discharge port of the secondary horizontal crystallization tube is connected to the feed port of the secondary discharge valve through a pipeline, the discharge port of the secondary discharge valve is connected to the feed port of the secondary filter through a pipeline, one discharge port of the secondary filter is connected to the feed port of the secondary filter cake silo through a pipeline, and the other discharge port of the secondary filter is connected to the feed port of the secondary filtrate receiving tank through a pipeline.

[0013] Preferably: the first-level horizontal crystallization tube includes a tube body, a first-level driving shaft is arranged in the tube body, the first-level driving shaft is a screw conveyor, which can push the material forward in the tube body, and a jacket is arranged on the outside of the tube body, and the jacket is connected to the first-level cooling system through a pipeline.

[0014] Technical effects and advantages of the utility model:

[0015] In the utility model, the raw material is crystallized in a first-level horizontal crystallization tube, a first-level cooling system is turned on, and then the raw material is pumped into a second-level horizontal crystallization tube, and the second-level cooling system is turned on to achieve gradient cooling, increase product crystallinity, and achieve efficient crystallization and rapid output of the product. BRIEF DESCRIPTION OF THE DRAWINGS

[0016] Figure 1 This is a schematic diagram of the structure of a crystallization device for producing lithium difluorooxalate borate provided in an embodiment of the present application;

[0017] Figure 2 It is a structural schematic diagram of a primary cooling system in a crystallization device for producing lithium difluorooxalate borate provided in an embodiment of the present application.

[0018] In the figure: 1. primary feed valve; 2. primary feed bin; 3. primary transfer pump; 4. primary horizontal crystallization tube; 41. tube body; 42. primary driving shaft; 43. jacket; 5. primary cooling system; 6. primary discharge valve; 7. primary filter; 8. primary filter cake silo; 9. primary filtrate transfer tank; 10. transfer transfer pump; 11. scraper; 12. heating system; 13. solvent condenser; 14. solvent receiving tank; 15. secondary feed bin; 16. secondary transfer pump; 17. secondary horizontal crystallization tube; 18. secondary cooling system; 19. secondary discharge valve; 20. secondary filter; 21. secondary filter cake silo; 22. secondary filtrate receiving tank. DETAILED DESCRIPTION

[0019] The present invention is further described in detail below in conjunction with the accompanying drawings and specific embodiments. The embodiments of the present invention are provided for the purpose of illustration and description, and are not intended to be exhaustive or to limit the present invention to the disclosed forms. Many modifications and variations are obvious to those of ordinary skill in the art. The embodiments are selected and described in order to better illustrate the principles and practical applications of the present invention, and to enable those of ordinary skill in the art to understand the present invention and thereby design various embodiments with various modifications suitable for specific purposes.

[0020] See also Figure 1 As shown, in this embodiment, a crystallization device for producing lithium difluorooxalate borate is provided, including a primary horizontal crystallization tube 4 and a secondary horizontal crystallization tube 17. The primary horizontal crystallization tube 4 and the secondary horizontal crystallization tube 17 have the same structural design. The primary horizontal crystallization tube 4 is connected to the primary cooling system 5, and the secondary horizontal crystallization tube 17 is connected to the secondary cooling system 18. The material is crystallized through the primary horizontal crystallization tube 4, the primary cooling system 5 is turned on, and then pumped into the secondary horizontal crystallization tube 17, and the secondary cooling system 18 is turned on to achieve gradient cooling, increase the crystallinity of the product, and achieve efficient crystallization and rapid output of the product.

[0021] In this embodiment, the feed port of the first-level horizontal crystallization tube 4 is connected to the discharge port of the first-level transfer pump 3 through a pipeline, the feed port of the first-level transfer pump 3 is connected to the discharge port of the first-level feed bin 2 through a pipeline, the feed port of the first-level feed bin 2 is connected to the discharge port of the first-level feed valve 1 through a pipeline, and the feed port of the first-level feed valve 1 is connected to an external pipeline, and the material is transported into the crystallization equipment through the external pipeline.

[0022] Specifically, the primary feed valve 1 is opened, and after the lithium difluorooxalate borate solution enters the primary feed bin 2, the lithium difluorooxalate borate solution is pumped into the primary horizontal crystallization tube 4 through the primary transfer pump 3, and the temperature of the primary cooling system 5 is controlled. At the same time, the material moves forward in the primary horizontal crystallization tube 4, and the material is precipitated in the primary horizontal crystallization tube 4.

[0023] In this embodiment, the discharge port of the first-level horizontal crystallization tube 4 is connected to the feed port of the first-level discharge valve 6 through a pipeline, the discharge port of the first-level discharge valve 6 is connected to the first-level filter 7 through a pipeline, the material after the first crystallization is filtered by the first-level filter 7, one discharge port of the first-level filter 7 is connected to the first-level filter cake silo 8, and the other discharge port of the first-level filter 7 is connected to the feed port of the first-level filtrate transfer tank 9.

[0024] Specifically, the precipitated material passes through the primary discharge valve 6 and enters the primary filter 7 , the filtered solid is discharged to the primary filter cake silo 8 , and the filtrate enters the primary filtrate transfer tank 9 .

[0025] In this embodiment, the discharge port of the primary filtrate transfer tank 9 is connected to the feed port of the transfer transfer pump 10 through a pipeline, the discharge port of the transfer transfer pump 10 is connected to the feed port of the scraper 11 through a pipeline, one discharge port of the scraper 11 is connected to the feed port of the solvent condenser 13 through a pipeline, the discharge port of the solvent condenser 13 is connected to the feed port of the solvent receiving tank 14 through a pipeline, the scraper 11 is also connected to the heating system 12, and the other discharge port of the scraper 11 is connected to the feed port of the secondary feed bin 15 through a pipeline.

[0026] Specifically, the filtered mother liquor is pumped into the scraper 11 through the transfer pump 10, and the heating system 12 is turned on to evaporate the scraper under normal pressure. The evaporated solvent enters the solvent receiving tank 14 through the solvent condenser 13, and the concentrated material enters the secondary feed bin 15.

[0027] In this embodiment, the discharge port of the secondary feed bin 15 is connected to the feed port of the secondary transfer pump 16 through a pipeline, the discharge port of the secondary transfer pump 16 is connected to the feed port of the secondary horizontal crystallization tube 17 through a pipeline, the discharge port of the secondary horizontal crystallization tube 17 is connected to the feed port of the secondary discharge valve 19 through a pipeline, the secondary horizontal crystallization tube 17 is connected to the secondary cooling system 18, the discharge port of the secondary discharge valve 19 is connected to the feed port of the secondary filter 20 through a pipeline, one discharge port of the secondary filter 20 is connected to the feed port of the secondary filter cake bin 21 through a pipeline, and the other discharge port of the secondary filter 20 is connected to the feed port of the secondary filtrate receiving tank 22 through a pipeline.

[0028] Specifically, the concentrated material in the secondary feed bin 15 is pumped from the secondary transfer pump 16 into the secondary horizontal crystallization tube 17, the secondary cooling system 18 is turned on, the material moves forward in the secondary horizontal crystallization tube 17, and at the same time the material precipitates in the secondary horizontal crystallization tube 17, the precipitated material further moves forward through the secondary discharge valve 19, and enters the secondary filter 20, the filtered solid is discharged into the secondary filter cake bin 21 and then transferred to the drying station, the filtrate enters the secondary filtrate receiving tank 22 and then transferred to the mother liquor recovery station.

[0029] See also Figure 2As shown, the first-stage horizontal crystallization tube 4 includes a tube body 41, a first-stage driving shaft 42 is arranged inside the tube body 41, and the first-stage driving shaft 42 is a screw conveyor that can push the material forward in the tube body 41. A jacket 43 is arranged on the outside of the tube body 41, and the jacket 43 is connected to the first-stage cooling system 5 through a pipeline.

[0030] Specifically, the cooling medium in the primary cooling system 5 flows in the gap between the jacket 43 and the tube body 41 to cool the material.

[0031] The primary cooling system 5, heating system 12 and secondary cooling system 18 in the present application are all prior art. The primary cooling system 5 and the secondary cooling system 18 can adopt water-cooled coolers or oil-water coolers, and the heating system 12 can adopt an instant electric heating system.

[0032] The working principle of the utility model is:

[0033] The primary feed valve 1 is opened, and the lithium difluorooxalate borate solution enters the primary feed bin 2, and then is pumped into the lithium difluorooxalate borate solution to the primary horizontal crystallization tube 4 through the primary transfer pump 3, and the temperature of the primary cooling system 5 is controlled, and the material moves forward in the primary horizontal crystallization tube 4, and at the same time, the material is precipitated in the primary horizontal crystallization tube 4, and the precipitated material passes through the primary discharge valve 6 and enters the primary filter 7, and the filtered solid is discharged to the primary filter cake bin 8, and the filtrate enters the primary filtrate transfer tank 9, and the filtered mother liquor is pumped into the scraper 11 through the transfer pump 10, and the heating system 12 is turned on, and the scraper evaporates at normal pressure, and the evaporated The solvent enters the solvent receiving tank 14 through the solvent condenser 13, and the concentrated material enters the secondary feed bin 15. The concentrated material in the secondary feed bin 15 is pumped from the secondary transfer pump 16 to the secondary horizontal crystallization tube 17, and the secondary cooling system 18 is turned on. The material moves forward in the secondary horizontal crystallization tube 17, and at the same time, the material precipitates in the secondary horizontal crystallization tube 17. The precipitated material further moves forward through the secondary discharge valve 19 and enters the secondary filter 20. The filtered solid is discharged to the secondary filter cake silo 21 and then transferred to the drying station. The filtrate enters the secondary filtrate receiving tank 22 and then transferred to the mother liquor recovery station.

[0034] Obviously, the described embodiments are only some embodiments of the present invention, not all embodiments. Based on the embodiments of the present invention, all other embodiments obtained by ordinary technicians in this field and related fields without creative work should fall within the scope of protection of the present invention. Structures, devices and operating methods not specifically described and explained in the present invention shall be implemented according to conventional means in the field unless otherwise specified and limited.

Claims

1. A crystallization device for producing lithium difluorooxalatoborate, characterized in that: The invention comprises a primary horizontal crystallization tube (4), a film scraper (11) and a secondary horizontal crystallization tube (17). The primary horizontal crystallization tube (4) is connected to a primary cooling system (5), the secondary horizontal crystallization tube (17) is connected to a secondary cooling system (18), and the film scraper (11) is connected to a heating system (12). After the material is crystallized in the primary horizontal crystallization tube (4), it enters the film scraper (11) for evaporation and concentration, and then is pumped into the secondary horizontal crystallization tube (17) for crystallization.

2. A crystallization device for producing lithium difluorooxalatoborate according to claim 1, characterized in that: The feed port of the first-stage horizontal crystallization tube (4) is connected to the discharge port of the first-stage transfer pump (3) through a pipeline, the feed port of the first-stage transfer pump (3) is connected to the discharge port of the first-stage feed bin (2) through a pipeline, the feed port of the first-stage feed bin (2) is connected to the discharge port of the first-stage feed valve (1) through a pipeline, and the feed port of the first-stage feed valve (1) is connected to an external pipeline.

3. A crystallization device for producing lithium difluorooxalatoborate according to claim 2, characterized in that: The discharge port of the first-stage horizontal crystallization tube (4) is connected to the feed port of the first-stage discharge valve (6) through a pipeline, and the discharge port of the first-stage discharge valve (6) is connected to the first-stage filter (7) through a pipeline.

4. A crystallization device for producing lithium difluorooxalatoborate according to claim 3, characterized in that: One discharge port of the primary filter (7) is connected to a primary filter cake silo (8), and another discharge port of the primary filter (7) is connected to a feed port of a primary filtrate transfer tank (9).

5. A crystallization device for producing lithium difluorooxalatoborate according to claim 4, characterized in that: The discharge port of the primary filtrate transfer tank (9) is connected to the feed port of the transfer transfer pump (10) through a pipeline, and the discharge port of the transfer transfer pump (10) is connected to the feed port of the scraper (11) through a pipeline.

6. A crystallization device for producing lithium difluorooxalatoborate according to claim 5, characterized in that: An outlet of the scraper (11) is connected to a feed port of a solvent condenser (13) through a pipeline, and an outlet of the solvent condenser (13) is connected to a feed port of a solvent receiving tank (14) through a pipeline.

7. A crystallization device for producing lithium difluorooxalatoborate according to claim 6, characterized in that: Another discharge port of the film scraper (11) is connected to a feed port of a secondary feed bin (15) via a pipeline.

8. A crystallization device for producing lithium difluorooxalatoborate according to claim 7, characterized in that: The discharge port of the secondary feed bin (15) is connected to the feed port of the secondary material transfer pump (16) through a pipeline, and the discharge port of the secondary material transfer pump (16) is connected to the feed port of the secondary horizontal crystallization tube (17) through a pipeline.

9. A crystallization device for producing lithium difluorooxalatoborate according to claim 8, characterized in that: The discharge port of the secondary horizontal crystallization tube (17) is connected to the feed port of the secondary discharge valve (19) through a pipeline, the discharge port of the secondary discharge valve (19) is connected to the feed port of the secondary filter (20) through a pipeline, one discharge port of the secondary filter (20) is connected to the feed port of the secondary filter cake silo (21) through a pipeline, and the other discharge port of the secondary filter (20) is connected to the feed port of the secondary filtrate receiving tank (22) through a pipeline.

10. A crystallization device for producing lithium difluorooxalatoborate according to claim 9, characterized in that: The first-stage horizontal crystallization tube (4) comprises a tube body (41), a first-stage driving shaft (42) is arranged inside the tube body (41), the first-stage driving shaft (42) is a screw conveyor, and can drive the material forward in the tube body (41), and a jacket (43) is arranged outside the tube body (41), and the jacket (43) is connected to the first-stage cooling system (5) through a pipeline.