CN212882481U

CN212882481U - Device for reducing insoluble substances in lithium hexafluorophosphate product

Info

Publication number: CN212882481U
Application number: CN202021082681.8U
Authority: CN
Inventors: 魏林埔; 张明; 谷洪闪
Original assignee: Dongying Shida Shenghua New Energy Co ltd; Shandong Shida Shenghua Chemical Group Co Ltd
Current assignee: Dongying Shida Shenghua New Energy Co ltd; Shinghwa Advanced Material Group Co Ltd
Priority date: 2020-06-12
Filing date: 2020-06-12
Publication date: 2021-04-06
Anticipated expiration: 2030-06-12

Abstract

The utility model relates to a reduce device of lithium hexafluorophosphate product insoluble. The technical scheme is as follows: the top of the double-layer sieve plate type reactor is provided with a phosphorus pentachloride solid feeding port, one side of the double-layer sieve plate type reactor is provided with a screw conveyor, the tail end of the screw conveyor is positioned above the phosphorus pentachloride solid feeding port, the left side of the double-layer sieve plate type reactor is provided with an anhydrous hydrogen fluoride gas pipeline, one side of the top of the double-layer sieve plate type reactor is provided with a reactor nitrogen pipeline, and the other side of the top of the double-layer sieve plate type reactor is provided with a phosphorus pentafluoride gas outlet pipeline. The beneficial effects are that: the utility model discloses a double-deck screen plate reactor can effectively improve the area of contact of hydrogen fluoride and phosphorus pentachloride to improve reaction efficiency greatly, produce the higher phosphorus pentafluoride of purity and participate in the synthesis reaction, also can shorten reaction time when reducing the hydrogen fluoride use amount, reduce insoluble content in the lithium hexafluorophosphate product.

Description

Device for reducing insoluble substances in lithium hexafluorophosphate product

Technical Field

The utility model relates to a lithium hexafluorophosphate production auxiliary device, in particular to reduce device of lithium hexafluorophosphate product undissolved substance.

Background

Lithium hexafluorophosphate is mainly used for manufacturing lithium ion batteries, is a core material of lithium ion electrolyte, has the advantages of good ionic conductivity, long cycle life, large energy ratio, small self-discharge, no memory effect, simple treatment, good environmental protection performance and the like, and is the preferred electrolyte of the current commercial lithium ion batteries. The process for producing the lithium hexafluorophosphate LiPF6 by using the anhydrous hydrogen fluoride as the solvent has the advantages of easy reaction, easy crystal separation of the product and easy realization of industrialization, and is a mature production process route at present. The process is mainly characterized in that gaseous hydrogen fluoride and phosphorus pentachloride solid react to generate phosphorus pentafluoride, and the generated phosphorus pentafluoride gas is introduced into a hydrogen fluoride solution containing lithium fluoride to react the phosphorus pentafluoride and the lithium fluoride to generate the lithium hexafluorophosphate. And then, by utilizing the solubility difference of lithium hexafluorophosphate at different temperatures, carrying out static crystallization by adopting stepwise cooling to below-40 ℃, and separating out lithium hexafluorophosphate solid. The content of insoluble substances in the product is directly influenced by the effect of the lithium hexafluorophosphate synthesis reaction, wherein the phosphorus pentafluoride reaction accounts for the main factor, the product quality can be effectively improved by improving the conversion rate of the phosphorus pentafluoride, and the content of the insoluble substances in the product is reduced.

Disclosure of Invention

The utility model aims at providing a reduce device of lithium hexafluorophosphate product insoluble substance to the above-mentioned defect that prior art exists, adopt double-deck sieve plate reactor can effectively improve the area of contact of hydrogen fluoride and phosphorus pentachloride to improve reaction efficiency greatly, produce the higher phosphorus pentafluoride of purity and participate in the synthetic reaction, also can shorten reaction time when reducing the hydrogen fluoride use amount, reduce insoluble substance content in the lithium hexafluorophosphate product.

The utility model provides a reduce device of lithium hexafluorophosphate product insoluble, its technical scheme is: including anhydrous hydrogen fluoride gas pipeline 1, phosphorus pentafluoride gas outlet pipeline 2, reactor nitrogen gas pipeline 3, screw conveyer 4, double-deck sieve plate reactor 5 and feed tank 7, double-deck sieve plate reactor 5's top is equipped with phosphorus pentachloride solid charge door 5.2, installs screw conveyer 4 in one side of double-deck sieve plate reactor 5, and screw conveyer 4's end is located phosphorus pentachloride solid charge door 5.2's top, is equipped with anhydrous hydrogen fluoride gas pipeline 1 in double-deck sieve plate reactor 5's left side, is equipped with reactor nitrogen gas pipeline 3 in double-deck sieve plate reactor 5's top one side, and the opposite side is equipped with phosphorus pentafluoride gas outlet pipeline 2.

Preferably, the double-layer sieve plate type reactor 5 comprises a gas anhydrous hydrogen fluoride feeding port 5.1, a phosphorus pentachloride solid feeding port 5.2, a gas phosphorus pentafluoride discharging port 5.3, a nitrogen gas feeding port 5.5, a reactor internal sieve plate 5.6, solid phosphorus pentachloride 5.7, a vent port 5.9 and a shell main body 5.10, two reaction cavities are separated from the shell main body 5.10 through the reactor internal sieve plate 5.6, the gas anhydrous hydrogen fluoride feeding ports 5.1 are respectively arranged and connected to the upper sides of the two reaction cavities through a gas transmission pipeline 5.11, the top of the shell main body 5.10 is provided with the phosphorus pentachloride solid feeding port 5.2, the gas phosphorus pentafluoride discharging port 5.3 and the nitrogen gas feeding port 5.5, and the bottom is provided with the vent port 5.9.

Preferably, a ventilation pipe 5.8 is arranged between two reaction cavities which are separated by a sieve plate 5.6 in the reactor.

Preferably, the top of the shell main body 5.10 is provided with a double-layer sieve plate type reactor standby port 5.4.

Preferably, the sieve plates 5.6 in the reactor are full of holes with different sizes, and the diameters of the holes are gradually reduced from the center of the sieve plate to the edge.

Preferably, air outlet holes are distributed on the lower side of the air transmission pipeline 5.11.

The utility model has the advantages that: the utility model adopts the dry nitrogen gas to completely replace, adds quantitative phosphorus pentafluoride into the double-layer sieve plate type reactor through the screw conveyer in a closed manner, then slowly introduces anhydrous hydrogen fluoride gas into the reactor, makes the anhydrous hydrogen fluoride gas react with phosphorus pentachloride to generate phosphorus pentafluoride gas, and enters a reaction working section for subsequently synthesizing lithium hexafluorophosphate;

the double-layer sieve plate type reactor can effectively improve the contact area of hydrogen fluoride and phosphorus pentachloride, thereby greatly improving the reaction efficiency, generating phosphorus pentafluoride with higher purity to participate in the synthesis reaction, shortening the reaction time while reducing the usage amount of hydrogen fluoride and reducing the content of insoluble substances in lithium hexafluorophosphate products.

Drawings

FIG. 1 is a schematic structural diagram of the present invention;

FIG. 2 is a schematic structural view of a double-deck sieve plate reactor;

FIG. 3 is a schematic structural view of a sieve plate inside the reactor;

in the upper diagram: an anhydrous hydrogen fluoride gas pipeline 1, a phosphorus pentafluoride gas outlet pipeline 2, a reactor nitrogen pipeline 3, a screw conveyer 4, a double-layer sieve plate type reactor 5, a motor 6 and a feeding tank 7,

the device comprises a gas anhydrous hydrogen fluoride feeding port 5.1, a phosphorus pentachloride solid feeding port 5.2, a gas phosphorus pentafluoride discharging port 5.3, a double-layer sieve plate type reactor standby port 5.4, a nitrogen feeding port 5.5, a reactor internal sieve plate 5.6, solid phosphorus pentachloride 5.7, a ventilation pipeline 5.8, a vent port 5.9, a shell main body 5.10 and a gas transmission pipeline 5.11.

Detailed Description

The preferred embodiments of the present invention will be described in conjunction with the accompanying drawings, and it will be understood that they are presented herein only to illustrate and explain the present invention, and not to limit the present invention.

Embodiment 1, refer to figure 1, the utility model provides a reduce device of lithium hexafluorophosphate product insoluble, including anhydrous hydrogen fluoride gas pipeline 1, phosphorus pentafluoride gas outlet pipeline 2, reactor nitrogen gas pipeline 3, screw conveyer 4, double-deck sieve plate reactor 5, motor 6 and feed tank 7, double-deck sieve plate reactor 5's top is equipped with phosphorus pentachloride solid charge door 5.2, installs screw conveyer 4 in one side of double-deck sieve plate reactor 5, and screw conveyer 4's end is located phosphorus pentachloride solid charge door 5.2's top, and screw conveyer 4 passes through the drive of motor 6, is equipped with anhydrous hydrogen fluoride gas pipeline 1 in double-deck sieve plate reactor 5's left side, is equipped with reactor nitrogen gas pipeline 3 in one side of double-deck sieve plate reactor 5's top, and the opposite side is equipped with phosphorus pentafluoride gas outlet pipeline 2.

Referring to the attached drawing 2, the double-deck sieve plate reactor 5 provided by the present invention comprises a gas anhydrous hydrogen fluoride feed inlet 5.1, a phosphorus pentachloride solid feed inlet 5.2, a gas phosphorus pentafluoride discharge port 5.3, a nitrogen feed inlet 5.5, a reactor internal sieve plate 5.6, a solid phosphorus pentachloride 5.7, a vent 5.9 and a shell main body 5.10, wherein two reaction cavities are separated from the shell main body 5.10 through the reactor internal sieve plate 5.6, the two reaction cavities are respectively provided with the gas anhydrous hydrogen fluoride feed inlet 5.1, the gas anhydrous hydrogen fluoride feed inlet is connected to the upper sides of the two reaction cavities through a gas transmission pipeline 5.11, the top of the shell main body 5.10 is provided with a phosphorus pentachloride solid feed inlet 5.2, a gas phosphorus pentafluoride discharge port 5.3, a nitrogen feed inlet 5.5, the bottom is provided with a vent 5.9, and the gas phosphorus pentafluoride discharge port 5.3 is communicated with the reaction cavities.

In addition, a vent pipe 5.8 is arranged between two reaction cavities separated by a sieve plate 5.6 in the reactor, gas can enter the inner cavity of the next layer to react, the mixing is more uniform, and the reaction is more sufficient.

The top of the shell main body 5.10 is provided with a double-layer sieve plate type reactor standby port 5.4, holes with different sizes are fully distributed on the sieve plate 5.6 in the reactor, the diameters of the holes are gradually reduced from the center of the sieve plate to the edge, so that phosphorus pentachloride powder can form a cone shape among the holes for accumulation, a small amount of powder falling into the lower layer through the holes can also form a cone shape for accumulation, and the surface area of the phosphorus pentachloride is greatly increased.

The lower side of the gas transmission pipeline 5.11 is provided with gas outlet holes, so that gas can be conveniently blown to the solid phosphorus pentachloride below, and the reaction is more complete.

The utility model discloses a theory of use as follows:

after the gas in the device is replaced by dry nitrogen, adding phosphorus pentachloride solid powder on a sieve plate from the upper part of a reactor through a screw conveyor, wherein the sieve plate is fully distributed with holes with different sizes, and the holes are gradually and regularly reduced from the center of the sieve plate to the edge, so that the phosphorus pentachloride powder can form cone-shaped accumulation among the holes, and a small amount of powder falling into the lower layer through the holes can also form cone-shaped accumulation, thereby greatly increasing the surface area of the phosphorus pentachloride; then, the anhydrous hydrogen fluoride gas is conveyed to the inner cavity of the reactor, and the vent pipeline extends into the upper layer and the lower layer of the reactor, so that the entered hydrogen fluoride is uniformly diffused to the two inner cavities of the reactor, the contact area of the hydrogen fluoride and the phosphorus pentachloride is effectively increased, and the reaction efficiency is greatly improved; the generated gas phosphorus pentafluoride enters the subsequent synthesis reaction along the gas outlet channel penetrating into the second layer, and the gas outlet is arranged because the raw material hydrogen fluoride has lighter specific gravity than the generated hydrogen chloride and phosphorus pentafluoride, if the gas outlet is arranged above, the heavy hydrogen chloride and the heavy phosphorus pentafluoride are accumulated below and attached to the surface of the phosphorus pentafluoride, and the lighter hydrogen fluoride gas floats above and can not effectively react with the phosphorus pentafluoride, and can enter the subsequent working section along a pipeline to cause the waste of a large amount of unreacted raw materials, and the gas outlet can effectively avoid the problem after the arrangement, the generated phosphorus pentafluoride with higher purity participates in the synthesis reaction, so that the reaction time can be shortened while the usage amount of the hydrogen fluoride is reduced, and the content of insoluble substances in the lithium hexafluorophosphate product is reduced.

The above description is only a preferred embodiment of the present invention, and any person skilled in the art may modify the present invention or modify it into an equivalent technical solution by using the technical solutions described above. Therefore, any simple modifications or equivalent replacements made according to the technical solution of the present invention belong to the scope of the claimed invention as far as possible.

Claims

1. The utility model provides a reduce device of lithium hexafluorophosphate product insoluble, characterized by: including anhydrous hydrogen fluoride gas pipeline (1), phosphorus pentafluoride gas outlet pipeline (2), reactor nitrogen gas pipeline (3), screw conveyer (4), double-deck sieve plate-type reactor (5) and feed tank (7), the top of double-deck sieve plate-type reactor (5) is equipped with phosphorus pentachloride solid charge door (5.2), installs screw conveyer (4) in one side of double-deck sieve plate-type reactor (5), and the end of screw conveyer (4) is located the top of phosphorus pentachloride solid charge door (5.2), and the other end is equipped with the below of installing at feed tank (7), is equipped with anhydrous hydrogen fluoride gas pipeline (1) in the left side of double-deck sieve plate-type reactor (5), is equipped with reactor nitrogen gas pipeline (3) in top one side of double-deck sieve plate-type reactor (5), and the opposite side is equipped with phosphorus pentafluoride gas outlet pipeline (2).

2. The apparatus for reducing insolubles in lithium hexafluorophosphate product of claim 1, wherein: the double-layer sieve plate type reactor (5) comprises a gas anhydrous hydrogen fluoride feeding hole (5.1), a phosphorus pentachloride solid feeding hole (5.2), a gas phosphorus pentafluoride discharging hole (5.3), a nitrogen feeding hole (5.5), a reactor internal sieve plate (5.6), solid phosphorus pentachloride (5.7), a vent hole (5.9) and a shell main body (5.10), wherein the shell main body (5.10) is internally provided with two reaction inner cavities which are separated through the reactor internal sieve plate (5.6), the gas anhydrous hydrogen fluoride feeding hole (5.1) is respectively arranged and is connected to the upper sides of the two reaction inner cavities through a gas transmission pipeline (5.11), the top of the shell main body (5.10) is provided with the phosphorus pentachloride solid feeding hole (5.2), the gas phosphorus pentafluoride discharging hole (5.3) and the nitrogen feeding hole (5.5), and the bottom of the shell main body is provided with the vent hole (5.9).

3. The apparatus for reducing insolubles in lithium hexafluorophosphate product according to claim 2, wherein: an air duct (5.8) is arranged between two reaction cavities separated by a sieve plate (5.6) in the reactor.

4. The apparatus for reducing insolubles in lithium hexafluorophosphate product according to claim 2, wherein: the top of the shell main body (5.10) is provided with a standby port (5.4) of the double-layer sieve plate type reactor.

5. The apparatus for reducing insolubles in lithium hexafluorophosphate product according to claim 2 or 3, wherein: the inside sieve (5.6) of reactor on be covered with the hole of not uniform size, the diameter of hole diminishes to the edge one by one from the sieve center.

6. The apparatus for reducing insolubles in lithium hexafluorophosphate product according to claim 2, wherein: and air outlet holes are distributed on the lower side of the air transmission pipeline (5.11).