Device for reducing content of chloride ions in lithium difluoro (oxalato) borate

By using a device to reduce chloride ion content in the production process of diefluorosate, use nitrogen anti -blowing technology and tail gas treatment device to treat moisture and chloride ions, and combined with the exhaust system of the rake dryer to solve the ion ion content does not fail the content The problem of stability improves product quality and stability.

CN222400347UActive Publication Date: 2025-01-28DONGGUAN UPC IND & TRADE
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Patent Information

Application Number
CN202323348637.3
Authority / Receiving Office
CN · China
Patent Type
Utility models(China)
Current Assignee / Owner
Filing Date
2023-12-08
Publication Date
2025-01-28
Estimated Expiration
2033-12-08

AI Technical Summary

Technical Problem

In the production process of lithium difluoroxalate borate, silicon tetrachloride is used in the raw materials, which leads to chloride ions brought into the synthetic product, resulting in unstable chloride ion content, exceeding the product's index requirements and affecting product quality.

Method used

A device that reduces the chlorine ion content in lithium diofluorophone boric acid, including nitrogen storage tank, flow regulating valve, gas pipeline, nitrogen spray room, nitrogen anti -blow storage tank, nitrogen blowing pipe, acid gas neutral and tail gas, tail gas, tail gas The processing device, filter filter, rake dryer, etc., carry water and chloride ion to process through nitrogen anti -blowing technology and tail gas treatment device, and completely draw the remaining chloride ion with the exhaust system that combines the rake dryer.

Benefits of technology

Effectively reduce the content of chloride ions in lithium diofluorophobolic acid, control it within the scope of the indicator, improve the quality of the product, and ensure the stability of the product and meet the standards.

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Abstract

The utility model relates to a device for reducing the content of chloride ions in lithium difluoro (oxalato) borate. According to the technical scheme, a lithium difluoro (oxalato) borate synthetic liquid tank is connected to the middle side of a nitrogen back flushing storage tank through a pipeline and a material conveying pump, a nitrogen spraying chamber is arranged above the top of the nitrogen back flushing storage tank, the lower portion of the nitrogen spraying chamber is connected with a nitrogen blowing pipe, and one side of the nitrogen spraying chamber is communicated to a nitrogen storage tank through a gas conveying pipeline; the upper side of the nitrogen back flushing storage tank is connected with the acid gas neutralization tank and the tail gas treatment device through pipelines, the bottom of the nitrogen back flushing storage tank is connected to the filter press through a material conveying pipeline, and the output end of the filter press is connected to a feed port of the rake dryer. The device has the beneficial effects that by utilizing a nitrogen back flushing technology, acid in a synthetic liquid is carried to be fed into the acid gas neutralization tank for pretreatment and then is fed into the tail gas treatment device, and in addition, residual chloride ions in lithium difluoro (oxalato) borate are completely extracted through an air extraction system of the rake type drying machine, so that the product quality is improved.
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Description

Technical Field

[0001] The utility model relates to an auxiliary device for preparing lithium difluorooxalate borate, in particular to a device for reducing the chloride ion content in lithium difluorooxalate borate. Background Art

[0002] In the preparation of lithium-ion batteries, the composition and properties of lithium salts in lithium-ion battery electrolytes also play an important role in the comprehensive electrochemical performance of lithium-ion batteries. Among them, lithium difluorooxalate borate has excellent high and low temperature performance, a wide operating temperature range, and good thermal stability. It can be used as a film-forming additive in lithium-ion battery electrolytes, or replace lithium hexafluorophosphate as an electrolyte salt. However, in the production process of lithium difluorooxalate borate, silicon tetrachloride is used as a raw material, which brings chloride ions into the synthetic product. Due to the certain deviation in the amount of addition, the chloride ions in the product detection show unstable data, sometimes <5.0ppm, sometimes >10.0ppm, which exceeds the product index requirements and affects the product quality. Utility Model Content

[0003] The purpose of the utility model is to provide a device for reducing the chloride ion content in lithium difluorooxalate borate in view of the above-mentioned defects in the prior art, so that the chloride ion content is less than 5.0ppm, thereby controlling the chloride ion content in lithium difluorooxalate borate within the index range and improving the quality of the product.

[0004] The utility model discloses a device for reducing the chloride ion content in lithium difluorooxalate borate, and the technical scheme thereof is as follows: comprising a nitrogen storage tank (1), a flow regulating valve (3), a gas transmission pipeline (5), a bracket (6), a nitrogen spray chamber (7), a nitrogen backflush storage tank (8), a nitrogen blowing pipe (9), an acid gas neutralization tank (10), an exhaust gas treatment device (11), a filter press (12), a rake dryer (13), a lithium difluorooxalate borate finished product container (14), a feed pipeline (15), a filter press discharge pipe (16), a lithium difluorooxalate borate synthetic liquid tank (17), and a feed pump (18), wherein the lower end of the lithium difluorooxalate borate synthetic liquid tank (17) is connected to the middle side of the nitrogen backflush storage tank (8) through a pipeline and a feed pump (18), and the top of the nitrogen backflush storage tank (8) is connected to the lower end of the lithium difluorooxalate borate synthetic liquid tank (17). A nitrogen spray chamber (7) is provided, the nitrogen spray chamber (7) is installed on a bracket (6), and the lower part of the nitrogen spray chamber (7) is connected to the inner cavity of a nitrogen backflush storage tank (8) through one or more nitrogen blowing pipes (9), and one side of the nitrogen spray chamber (7) is connected to the nitrogen storage tank (1) through a gas transmission pipeline (5) and a flow regulating valve (3); the upper side of the nitrogen backflush storage tank (8) is connected to an acid gas neutralization tank (10) and an exhaust gas treatment device (11) through a pipeline, the bottom of the nitrogen backflush storage tank (8) is connected to a filter press (12) through a material transmission pipeline (15), and the output end of the filter press (12) is connected to the feed port of a rake dryer (13) through a filter press discharge pipe (16), and a lithium difluorooxalate borate finished product container (14) is placed below the discharge port of the rake dryer (13).

[0005] Preferably, the nitrogen backflush storage tank (8) is mounted on the second base (21), and the rear end of the second base (21) is fixedly connected to the bracket (6).

[0006] Preferably, the flow regulating valve (3) is mounted on the first base (4), and the flow regulating valve (3) is connected to a pressure gauge (2).

[0007] Preferably, one side of the acid gas neutralization tank (10) is connected to the nitrogen backflush storage tank (8) via a pipeline, and the other side is connected to the tail gas treatment device (11) via a pipeline.

[0008] Preferably, a first control valve (19) is provided at the discharge port at the lower end of the lithium difluorooxalate borate synthesis liquid tank (17), and a second control valve (20) is installed at the output end of the feed pump (18).

[0009] Preferably, the lower end outlet of the nitrogen blowing pipe (9) is located below the liquid level of lithium difluorooxalate borate in the inner cavity of the nitrogen backflush storage tank (8).

[0010] Preferably, the lower end of the nitrogen blowing pipe (9) is connected to a blowing head (a), and the blowing head (a) comprises an upper joint (a1) of the nitrogen blowing pipe, a knob (a2), a conical tube (a3), and a lower outlet (a4); the upper end of the conical tube (a3) ​​is connected to the upper joint (a1) of the nitrogen blowing pipe through the knob (a2), and a lower outlet (a4) is provided at the lower end of the conical tube (a3).

[0011] The beneficial effects of the utility model are as follows: the utility model utilizes nitrogen back-blowing technology to carry acid in the synthetic liquid into the acid gas neutralization tank for pretreatment, and then sends it to the tail gas treatment device, which is conducive to carrying moisture and chloride ions into the tail gas treatment device, thereby reducing the chloride ion content of the lithium difluorooxalate borate product; in addition, the remaining chloride ions of the lithium difluorooxalate borate are completely extracted by using the exhaust system of the rake dryer, and then the material is fully dried, thereby reducing the chloride ion content in the material and improving the product quality. BRIEF DESCRIPTION OF THE DRAWINGS

[0012] Figure 1 It is a structural schematic diagram of the utility model;

[0013] Figure 2 It is a schematic diagram of the structure of the air blowing head;

[0014] In the figure above: nitrogen storage tank 1, pressure gauge 2, flow regulating valve 3, first base 4, gas pipeline 5, bracket 6, nitrogen spray chamber 7, nitrogen backflush storage tank 8, nitrogen blowing pipe 9, acid gas neutralization tank 10, tail gas treatment device 11, filter press 12, rake dryer 13, lithium difluoro oxalate borate finished product container 14, feed pipeline 15, filter press discharge pipe 16, lithium difluoro oxalate borate synthetic liquid tank 17, feed pump 18, first control valve 19, second control valve 20, second base 21, blowing head a, nitrogen blowing pipe upper joint a1, knob a2, tapered tube a3, lower outlet a4 DETAILED DESCRIPTION

[0015] The preferred embodiments of the present invention are described below in conjunction with the accompanying drawings. It should be understood that the preferred embodiments described herein are only used to illustrate and explain the present invention, and are not used to limit the present invention.

[0016] Example 1, reference Figure 1The utility model mentions a device for reducing the chloride ion content in lithium difluorooxalate borate, comprising a nitrogen storage tank 1, a flow regulating valve 3, a gas transmission pipeline 5, a bracket 6, a nitrogen spray chamber 7, a nitrogen backflush storage tank 8, a nitrogen blowing pipe 9, an acid gas neutralization tank 10, a tail gas treatment device 11, a filter press 12, a rake dryer 13, a lithium difluorooxalate borate finished product container 14, a feed pipeline 15, a filter press discharge pipe 16, a lithium difluorooxalate borate synthetic liquid tank 17, and a feed pump 18. The lower end of the lithium difluorooxalate borate synthetic liquid tank 17 is connected to the middle side of the nitrogen backflush storage tank 8 through a pipeline and a feed pump 18. The top of the nitrogen backflush storage tank 8 is provided with A nitrogen spray chamber 7 is installed on a bracket 6, and the lower part of the nitrogen spray chamber 7 is connected to the inner cavity of a nitrogen back-blowing storage tank 8 through one or more nitrogen blowing pipes 9, and one side of the nitrogen spray chamber 7 is connected to the nitrogen storage tank 1 through a gas transmission pipeline 5 and a flow regulating valve 3; the upper side of the nitrogen back-blowing storage tank 8 is connected to an acid gas neutralization tank 10 and a tail gas treatment device 11 through a pipeline, and the bottom of the nitrogen back-blowing storage tank 8 is connected to a filter press 12 through a feed pipeline 15, and the output end of the filter press 12 is connected to the feed port of a rake dryer 13 through a filter press discharge pipe 16, and a lithium difluorooxalate borate finished product container 14 is placed below the discharge port of the rake dryer 13.

[0017] The nitrogen backflush storage tank 8 is installed on the second base 21 , and the rear end of the second base 21 is fixedly connected to the bracket 6 .

[0018] The flow regulating valve 3 is installed on the first base 4 , and the flow regulating valve 3 is connected to the pressure gauge 2 .

[0019] One side of the acid gas neutralization tank 10 is connected to the nitrogen backflush storage tank 8 through a pipeline, and the other side is connected to the tail gas treatment device 11 through a pipeline.

[0020] A first control valve 19 is provided at the discharge port at the lower end of the lithium difluorooxalate borate synthesis liquid tank 17 , and a second control valve 20 is installed at the output end of the feed pump 18 .

[0021] The lower end outlet of the nitrogen blowing pipe 9 is located below the liquid level of lithium difluorooxalate borate in the inner cavity of the nitrogen back-blowing storage tank 8 .

[0022] When the utility model is used, the lithium difluoro oxalate borate in the lithium difluoro oxalate borate synthesis liquid tank 17 is pumped into the nitrogen backflush storage tank 8 through the feed pump 18, and then the nitrogen blowing pipe 9 connected with the blowing head a is sent into the inner cavity of the nitrogen backflush storage tank 8, and the upper end is connected to the nitrogen spray chamber 7; then, the flow regulating valve 3 connected to the nitrogen storage tank 1 is opened, and the nitrogen is sent into the nitrogen backflush storage tank 8, and the nitrogen feeding amount is 0.5-1.0m3 / h; in addition, the upper side of the nitrogen backflush storage tank 8 is connected to the acid gas neutralization tank 10 and the tail gas treatment device 11 through a pipeline, and the acid gas and tail gas are treated by the acid gas neutralization tank 10; Observe the drop in the liquid level in the nitrogen backflush storage tank 8. If it drops too fast, such as 10 mm / h, adjust and reduce the nitrogen introduction amount, maintain the nitrogen introduction time for 12 hours, take samples to detect the chloride ion content in the difluoro oxalate lithium borate synthetic liquid, and after passing the test, send the difluoro oxalate lithium borate synthetic liquid in the nitrogen backflush storage tank 8 to the filter press 12 for treatment, and the product after filter pressure is sent to the rake dryer 13 for drying treatment, and the exhaust system of the rake dryer is used to completely extract the remaining chloride ions of the difluoro oxalate lithium borate, and the material is fully dried to reduce the chloride ion content in the material and improve the product quality.

[0023] Embodiment 2, the utility model mentioned a device for reducing the chloride ion content in lithium difluorooxalate borate, comprising a nitrogen storage tank 1, a flow regulating valve 3, a gas pipeline 5, a bracket 6, a nitrogen spray chamber 7, a nitrogen backflush storage tank 8, a nitrogen blowing pipe 9, an acid gas neutralization tank 10, a tail gas treatment device 11, a filter press 12, a rake dryer 13, a lithium difluorooxalate borate finished product container 14, a feed pipeline 15, a filter press discharge pipe 16, a lithium difluorooxalate borate synthetic liquid tank 17, and a feed pump 18, wherein the lower end of the lithium difluorooxalate borate synthetic liquid tank 17 is connected to the middle side of the nitrogen backflush storage tank 8 through a pipeline and a feed pump 18, and the top of the nitrogen backflush storage tank 8 is connected to the middle side of the nitrogen backflush storage tank 8. A nitrogen spray chamber 7 is provided, which is installed on a bracket 6, and the lower part of the nitrogen spray chamber 7 is connected to the inner cavity of a nitrogen back-blowing storage tank 8 through one or more nitrogen blowing pipes 9, and one side of the nitrogen spray chamber 7 is connected to the nitrogen storage tank 1 through a gas transmission pipeline 5 and a flow regulating valve 3; the upper side of the nitrogen back-blowing storage tank 8 is connected to an acid gas neutralization tank 10 and a tail gas treatment device 11 through a pipeline, and the bottom of the nitrogen back-blowing storage tank 8 is connected to a filter press 12 through a feed pipeline 15, and the output end of the filter press 12 is connected to the feed port of a rake dryer 13 through a filter press discharge pipe 16, and a lithium difluorooxalate borate finished product container 14 is placed below the discharge port of the rake dryer 13.

[0024] The difference from Example 1 is:

[0025] Reference Figure 2The lower end of the nitrogen blowing pipe 9 mentioned in the utility model is connected to the blowing head a, and the blowing head a includes a nitrogen blowing pipe upper joint a1, a knob a2, a conical tube a3, and a lower outlet a4. The upper end of the conical tube a3 is connected to the nitrogen blowing pipe upper joint a1 through the knob a2, and a lower outlet a4 is provided at the lower end of the conical tube a3. The blown nitrogen can be pressurized through the conical tube a3, thereby improving the backblowing effect; the blowing head a can be conveniently and quickly installed through the knob a2.

[0026] The above is only a preferred embodiment of the utility model. Any person skilled in the art may modify the utility model by using the above technical solution or modify it into an equivalent technical solution. Therefore, any simple modification or equivalent transformation based on the technical solution of the utility model shall fall within the scope of protection claimed by the utility model.

Claims

1. A device for reducing the chloride ion content in lithium difluorooxalate borate, characterized in that: The invention comprises a nitrogen storage tank (1), a flow regulating valve (3), a gas transmission pipeline (5), a bracket (6), a nitrogen spray chamber (7), a nitrogen backflush storage tank (8), a nitrogen blowing pipe (9), an acid gas neutralization tank (10), an exhaust gas treatment device (11), a filter press (12), a rake dryer (13), a lithium difluorooxalate borate finished product container (14), a feed pipeline (15), a filter press discharge pipe (16), a lithium difluorooxalate borate synthetic liquid tank (17), and a feed pump (18). The lower end of the lithium difluorooxalate borate synthetic liquid tank (17) is connected to the middle side of the nitrogen backflush storage tank (8) through a pipeline and a feed pump (18). A nitrogen spray chamber (7) is provided above the top of the nitrogen backflush storage tank (8). The nitrogen spray chamber (7) is arranged The nitrogen spray chamber (7) is mounted on a bracket (6), and the lower part of the nitrogen spray chamber (7) is connected to the inner cavity of the nitrogen backflush storage tank (8) through one or more nitrogen blowing pipes (9). One side of the nitrogen spray chamber (7) is connected to the nitrogen storage tank (1) through a gas transmission pipeline (5) and a flow regulating valve (3); the upper side of the nitrogen backflush storage tank (8) is connected to the acid gas neutralization tank (10) and the tail gas treatment device (11) through a pipeline, the bottom of the nitrogen backflush storage tank (8) is connected to the filter press (12) through a material transmission pipeline (15), and the output end of the filter press (12) is connected to the feed port of the rake dryer (13) through a filter press discharge pipe (16), and a lithium difluorooxalate borate finished product container (14) is placed below the discharge port of the rake dryer (13).

2. The device for reducing the chloride ion content in lithium difluorooxalatoborate according to claim 1, characterized in that: The nitrogen backflush storage tank (8) is mounted on the second base (21), and the rear end of the second base (21) is fixedly connected to the bracket (6).

3. The device for reducing the chloride ion content in lithium difluorooxalate borate according to claim 1 or 2, characterized in that: The flow regulating valve (3) is mounted on the first base (4), and the flow regulating valve (3) is connected to a pressure gauge (2).

4. The device for reducing the chloride ion content in lithium difluorooxalate borate according to claim 3, characterized in that: One side of the acid gas neutralization tank (10) is connected to the nitrogen backflush storage tank (8) via a pipeline, and the other side is connected to the tail gas treatment device (11) via a pipeline.

5. The device for reducing the chloride ion content in lithium difluorooxalate borate according to claim 4, characterized in that: A first control valve (19) is provided at the discharge port at the lower end of the lithium difluorooxalate borate synthesis liquid tank (17), and a second control valve (20) is installed at the output end of the feed pump (18).

6. The device for reducing chloride ion content in lithium difluorooxalate borate according to claim 5, characterized in that: The lower end outlet of the nitrogen blowing pipe (9) is located below the liquid level of lithium difluorooxalate borate in the inner cavity of the nitrogen back-blowing storage tank (8).

7. The device for reducing the chloride ion content in lithium difluorooxalate borate according to claim 6, characterized in that: The lower end of the nitrogen blowing pipe (9) is connected to the blowing head (a), and the blowing head (a) comprises an upper joint (a1) of the nitrogen blowing pipe, a knob (a2), a conical tube (a3), and a lower outlet (a4); the upper end of the conical tube (a3) ​​is connected to the upper joint (a1) of the nitrogen blowing pipe via the knob (a2), and a lower outlet (a4) is provided at the lower end of the conical tube (a3).