CN218088970U - Phosphorus pentafluoride gas generator - Google Patents
Phosphorus pentafluoride gas generator Download PDFInfo
- Publication number
- CN218088970U CN218088970U CN202222001109.XU CN202222001109U CN218088970U CN 218088970 U CN218088970 U CN 218088970U CN 202222001109 U CN202222001109 U CN 202222001109U CN 218088970 U CN218088970 U CN 218088970U
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- hydrogen fluoride
- liquid hydrogen
- generator
- cylinder
- phosphorus pentafluoride
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The utility model provides a phosphorus pentafluoride gas generator, be provided with 2 on the last barrel of its generator barrel and be used for adding liquid hydrogen fluoride to the liquid material feeder in the generator barrel, the lower barrel of generator barrel has along the liquid hydrogen fluoride infiltration clamp cover that the barrel inner wall set up down, and this liquid hydrogen fluoride infiltration clamp cover has and is used for bearing and contacts the isolation filter plate of phosphorus pentachloride solid material in the generator barrel supplies with liquid hydrogen fluoride through liquid hydrogen fluoride feeding mechanism, permeates the generator barrel through keeping apart the filter plate in, reacts with phosphorus pentachloride solid material. Adopt the utility model discloses a phosphorus pentafluoride gas generator can let the liquid hydrogen fluoride of participation reaction can be abundant with the phosphorus pentachloride solid material contact reaction of reaction object to improve the emergence efficiency of phosphorus pentafluoride gas.
Description
Technical Field
The utility model relates to a phosphorus pentafluoride gas generator, especially a required phosphorus pentafluoride gas generator when adopting hydrogen fluoride solvent method to synthesize lithium hexafluorophosphate for production.
Background
Lithium hexafluorophosphate serving as a key material lithium salt of the lithium ion battery is mainly applied to lithium ion electrolyte in two forms, namely crystalline lithium hexafluorophosphate and liquid lithium salt prepared with an organic solvent. At present, the lithium hexafluorophosphate crystal is sold in foreign markets, and the reasons are mainly that the lithium hexafluorophosphate crystal is beneficial to transportation and storage of products, has small potential safety hazard and is more matched with a process system of an electrolyte manufacturer. With the healthy continuous and steady development of new energy industry in China, the demand of the crystalline lithium hexafluorophosphate is increasing day by day, the production process of the crystalline lithium hexafluorophosphate is broken through and perfected, and the improvement of the quality of the crystalline lithium hexafluorophosphate product is the key point of the current domestic research.
At present, the preparation methods of lithium hexafluorophosphate mainly comprise the following steps: the gas-solid direct reaction method, the solvent method and the ion exchange method, wherein the hydrogen fluoride solvent method is the process which is most researched, the technology is the most mature and the industrial application is the most extensive. The existing hydrogen fluoride solvent method is to dissolve lithium salt in anhydrous hydrofluoric acid to form LiHF solution, and then to introduce phosphorus Pentafluoride (PF) 5 ) The gases react to produce lithium hexafluorophosphate. Namely, the process for preparing lithium hexafluorophosphate by using the hydrogen fluoride solvent method is a mature process at present and is a production method which is most easy to realize industrialization.
Specifically, the hydrogen fluoride solvent method is to utilize hydrogen fluoride as a reaction medium, dissolve raw material lithium halide in hydrogen fluoride, gasify high-purity phosphorus pentafluoride, introduce the gas into a solvent to react to generate lithium hexafluorophosphate crystals, and after the reaction is finished, obtain lithium hexafluorophosphate products through crystallization separation, drying and the like.
As a conventional phosphorus pentafluoride gas generator for producing phosphorus pentafluoride gas used for synthesizing lithium hexafluorophosphate by a hydrogen fluoride solvent method, there are two types, namely, a horizontal phosphorus pentafluoride gas generator and a vertical phosphorus pentafluoride gas generator, but in any of these phosphorus pentafluoride gas generators, a liquid transfer tube for introducing liquid hydrogen fluoride is inserted into a container of the generator, and the liquid hydrogen fluoride introduced through the liquid transfer tube reacts with a material (phosphorus pentafluoride solid) charged into the generator to produce a desired phosphorus pentafluoride gas.
In order to improve the contact chance between the liquid hydrogen fluoride and the phosphorus pentafluoride solid and improve the generation efficiency of the phosphorus pentafluoride gas, on one hand, the infusion tube is inserted into the generator more and more uniformly, and on the other hand, the stirring device is arranged in the generator to stir and reverse the phosphorus pentafluoride solid. That is, the phosphorus pentachloride solid material is contacted with liquid hydrogen fluoride while being stirred for reaction, so that the reaction can be more sufficient, and the amount of the generated phosphorus pentafluoride gas in unit time is increased. However, the number and distribution of the inserted infusion tubes can affect and limit the full stirring of the materials by the stirrer arranged in the generator, namely, the generator in the prior art has the problem that the gas generation efficiency of the generator is affected by sacrificing the contact opportunity of the liquid hydrogen fluoride and the phosphorus pentafluoride solid for preventing the infusion tubes and the stirrer from being put on a shelf.
Therefore, the technical field urgently needs a phosphorus pentafluoride gas generator which can lead the liquid hydrogen fluoride participating in the reaction to be fully contacted and reacted with the phosphorus pentachloride solid material of the reaction object, thereby improving the gas generation efficiency.
SUMMERY OF THE UTILITY MODEL
The utility model provides a pair of phosphorus pentafluoride gas generator, include: the device comprises a generator cylinder body, a stirring device, a liquid hydrogen fluoride supply device and a gas conveying pipeline, wherein the generator cylinder body consists of an upper cylinder body and a lower cylinder body, the stirring device is arranged in the generator cylinder body, the gas conveying pipeline is communicated with the generator cylinder body and is used for conveying phosphorus pentafluoride gas to a next process device, the upper cylinder body is provided with liquid material adding devices used for adding liquid hydrogen fluoride into the generator cylinder body, and each liquid material adding device is connected with the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline; the lower cylinder is provided with a liquid hydrogen fluoride permeation jacket arranged along the inner wall of the lower cylinder, the liquid hydrogen fluoride permeation jacket is provided with an isolation filter plate used for bearing and contacting the phosphorus pentachloride solid material in the generator cylinder, and the liquid hydrogen fluoride permeation jacket is connected with a liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline; the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket through the liquid hydrogen fluoride supply device permeates into the generator cylinder through the isolation filter plate and reacts with the phosphorus pentachloride solid material in the generator cylinder.
Preferably, the liquid hydrogen fluoride-permeable jacket, at least the separation filter plate thereof, is formed into a cone shape.
Preferably, the isolating filter plate adopts a plurality of layers of sintered filter screens.
Preferably, a cooling jacket is arranged on the outer wall of at least one of the upper cylinder and the lower cylinder, and the cooling jacket is connected with a cooling circulation device through a cooling medium conveying pipeline.
Further preferably, the stirring device has a hollow spiral belt, and the spiral belt is connected with the cooling circulation device.
Further preferably, a powder filter is disposed on the gas delivery pipeline.
Further preferably, a temperature transmitter is arranged in the generator cylinder, and a regulating valve is arranged on the cooling medium conveying pipeline.
According to the utility model discloses a phosphorus pentafluoride gas generator can let the liquid hydrogen fluoride who participates in the reaction can abundant and reaction object's phosphorus pentachloride solid material contact reaction to improve the emergence efficiency that phosphorus pentafluoride is gaseous.
Drawings
Fig. 1 shows a schematic structural view of a phosphorus pentafluoride gas generator of the present invention.
In the figure: 10-a phosphorus pentafluoride gas generator; 11-a generator cylinder; 12-a stirring device; 13-a solid material feeding device; 14-liquid hydrogen fluoride permeation jacket; 11 c-liquid material feeder; 14 a-an isolation filter plate; 20-liquid hydrogen fluoride supply means; 50-cooling circulation device.
Detailed Description
The technical solution and effects of the present invention will be described in detail below with reference to the embodiments. The following embodiments are merely illustrative of the present invention, and the present invention is not limited to the following embodiments or examples. Use the utility model discloses a think about right the utility model discloses the simple change that goes on is all in the utility model discloses the within range that claims.
The utility model discloses a phosphorus pentafluoride gas generator 10, as shown in fig. 1, has the agitating unit 12 that sets up in generator barrel 11 and this generator barrel 11.
The generator cylinder 11 is composed of an upper cylinder 11a and a lower cylinder 11 b. A solid material feeding device 13 is arranged on the upper cylinder 11a, and the solid material feeding device 13 comprises a hard seal ball valve 13a and a closed funnel 13b.
The upper cylinder 11a is provided with 2 sprayers 11c as a liquid material feeder for feeding liquid hydrogen fluoride into the generator cylinder 11, and each sprayer 11c is connected to a liquid hydrogen fluoride supply device 20 through a liquid hydrogen fluoride supply pipeline 11 d. The liquid material feeder is provided with a flow meter 11e and a regulating valve 11f.
The upper cylinder 11a is connected to the next process apparatus 30 through a gas transfer line 11g, and a powder filter 40 is provided on the gas transfer line 11 g. The next process apparatus 30 is, for example, a lithium hexafluorophosphate synthesizing system.
The lower cylinder 11b is provided with a liquid hydrogen fluoride permeation jacket 14 arranged along the inner wall of the lower cylinder 11b, the liquid hydrogen fluoride permeation jacket 14 is provided with an isolation filter plate 14a used for bearing and contacting phosphorus pentachloride solid materials in the generator cylinder 11, and the liquid hydrogen fluoride permeation jacket 14 is connected with the liquid hydrogen fluoride supply device 20 through a liquid hydrogen fluoride supply pipeline 14 b. In this embodiment, the liquid hydrogen fluoride supply line 14b is connected to another liquid hydrogen fluoride supply line 11 d.
In the present embodiment, the lower cylindrical body 11b is formed in a cone shape, and the diameter of the circumference of the bottom of the cone is substantially the same as the diameter of the upper cylindrical body 11a formed in a cylindrical shape, and the lower cylindrical body and the upper cylindrical body are integrally connected. The liquid hydrogen fluoride permeating jacket 14 is formed along the conical surface of the lower cylinder 11b, and the isolation filter plate 14a is formed into a conical shape. The isolating filter plate 14a adopts a plurality of layers of sintered filter screens. The liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeating jacket 14 by the liquid hydrogen fluoride supply device 20 permeates into the generator cylinder 11 through the isolation filter plate 14a, and reacts with the phosphorus pentachloride solid material in the generator cylinder 11, which is in contact with the isolation filter plate 14 a. The isolation filter plate 14a has a structure and characteristics that liquid hydrogen fluoride can permeate the isolation filter plate and phosphorus pentachloride solid materials can not pass through the isolation filter plate.
In addition, cooling jackets 15a, 15b are provided on the outer walls of the upper cylinder 11a and the lower cylinder 11b, respectively, and the cooling jackets 15a, 15b are connected to a cooling circulation device 50 through cooling medium transfer pipes 15c, 15 d. The cooling circulation device 50 includes a cooling medium supply device 50b and a cooling medium recovery device 50a. The cooling medium is supplied from the cooling medium supply device 50b through the cooling medium supply line 15d to the cooling jackets 15a and 15b, respectively, and then supplied from the cooling jackets 15a and 15b through the cooling medium supply line 15c to the cooling medium recovery device 50a. The cooling medium transfer line 15c is provided with a control valve 15e.
In addition, a hard sealing ball valve 16 for discharging unreacted phosphorus pentachloride solid material is arranged at the bottom of the lower cylinder body 11 b.
The stirring device 12 includes a helical blade 12a that rotates and stirs in the generator cylinder 11, and a driving motor 12b that drives the blade 12 a. The paddle 12a is hollow and connected to a cooling circulation device (not shown). During the stirring process, the temperature of the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride can be adjusted by introducing a temperature adjusting medium into the hollow paddle 12 a.
In addition, a temperature transmitter 60 is further provided in the generator cylinder 11, and the temperature change in the generator cylinder 11 is monitored by the temperature transmitter 60, so that the temperature in the generator cylinder 11 is adjusted and controlled in cooperation with the adjusting valve 15e.
The operation of the phosphorus pentafluoride gas generator of the present invention and the method of generating phosphorus pentafluoride gas using the same will be described below with reference to fig. 1.
As shown in FIG. 1, the driving motor 12b is first turned on to drive the paddle 12a to rotate, and then the phosphorus pentachloride solid material is added into the generator cylinder 11 through the hard sealing ball valve 13a and the closed funnel 13b. Specifically, the upper cover plates of the hard seal ball valve 13a and the closed funnel 13b are opened, the phosphorus pentachloride solid material is added into the generator cylinder 11 from the closed funnel 13b, and the upper cover plates of the hard seal ball valve 13a and the closed funnel 13b are closed after the addition is completed, so that the solid material adding process of adding the phosphorus pentachloride solid material into the generator cylinder 11 is finished.
Next, the liquid hydrogen fluoride is supplied from the liquid hydrogen fluoride supply device 20 through the flow meter 11e and the regulating valve 11f to the shower unit 11c through the liquid hydrogen fluoride supply line 11d, and is sprayed into the generator cylinder 11 through the shower unit 11 c. The pressure in the generator cylinder 11 is monitored by a pressure monitoring device, not shown, and when the pressure in the generator cylinder 11 reaches a predetermined pressure, liquid hydrogen fluoride is permeated and fed into the generator cylinder 11 through the liquid hydrogen fluoride permeation jacket 14. Namely, a liquid material charging process of charging liquid hydrogen fluoride into the generator cylinder 11 through the liquid material charger 11c and a liquid material permeating process of osmotically charging liquid hydrogen fluoride into the generator cylinder 11 through the liquid hydrogen fluoride permeating jacket 14 are performed.
In the above process, the temperature of the generator cylinder 11 is controlled by supplying a cooling medium to the cooling jackets 15a and 15b and circulating the cooling medium by the cooling circulation device 50, and at this time, the temperature change in the generator cylinder 11 is monitored by the temperature transmitter 60, and the temperature in the generator cylinder 11 is adjusted and controlled in cooperation with the adjustment valve 15e. On the other hand, in the stirring process, a temperature regulating medium is introduced into the hollow paddle 12a to regulate the temperature of the stirred phosphorus pentachloride solid material and the liquid hydrogen fluoride.
The phosphorus pentachloride gas generated by the reaction in the generator cylinder 11 is filtered by the powder filter 40, and then is transported to the next process device 30 through the gas transport pipeline 11 g.
And the unreacted phosphorus pentachloride solid material is discharged out of the generator cylinder body 11 through the hard sealing ball valve 16 for recycling.
Adopt the utility model discloses a phosphorus pentafluoride gas generator with come to take place phosphorus pentafluoride gas, have following advantage.
(1) The utility model discloses a setting has and is used for bearing and contacting the liquid hydrogen fluoride infiltration of the isolation filter plate 14a of the phosphorus pentachloride solid material in the generator barrel 11 presss from both sides cover 14 to the messenger passes through liquid hydrogen fluoride feeding mechanism 20 supplies with the liquid hydrogen fluoride of liquid hydrogen fluoride infiltration cover 14 permeates through isolating filter plate 14a and arrives in the generator barrel 11, with the phosphorus pentachloride solid material in the generator barrel 11 reacts. Therefore, the liquid hydrogen fluoride participating in the reaction can be fully contacted with the phosphorus pentachloride solid material of the reaction object for reaction, thereby improving the generation efficiency of the phosphorus pentafluoride gas.
(2) The liquid hydrogen fluoride permeation jacket 14 is provided with a conical isolation filter plate 14a, so that the contact area of the liquid hydrogen fluoride and the phosphorus pentachloride solid material can be increased.
(3) The cooling jackets 15a and 15b are arranged on the generator cylinder 11, the blades 12a of the stirring device 12 are also formed into a hollow shape, and the temperature and the reaction temperature of the phosphorus pentafluoride gas generator 10 in the process of generating the phosphorus pentafluoride gas can be controlled by a circulated cooling medium, so that the generation efficiency of the phosphorus pentafluoride gas is improved.
(4) The pressure in the generator cylinder 11 is adjusted by the liquid material feeding process, and when the pressure in the generator cylinder 11 reaches a predetermined pressure, liquid hydrogen fluoride is permeated and fed into the generator cylinder 11 through the liquid hydrogen fluoride permeation jacket 14. This can prevent the life of the isolation filter sheet 14a from being shortened or damaged due to an excessive difference between the pressure in the liquid hydrogen fluoride permeation jacket 14 and the pressure in the generator cylinder 11.
As a modification of the embodiment of the present invention, for example, a flow meter and a control valve may be provided in the liquid hydrogen fluoride supply line 14b to control the supply of the liquid hydrogen fluoride to the liquid hydrogen fluoride permeating jacket 14.
In addition, the number of the showers 11c as the liquid material feeder may be 1 or 3 or more.
The liquid hydrogen fluoride permeating jacket 14 and the isolation filter plate 14a may be formed in a shape other than a tapered shape.
It should be noted that the various features described in the above embodiments may be combined in any suitable manner without departing from the scope of the invention.
Claims (7)
1. A phosphorus pentafluoride gas generator comprising: a generator cylinder composed of an upper cylinder and a lower cylinder, a stirring device arranged in the generator cylinder, a liquid hydrogen fluoride supply device and a gas conveying pipeline communicated with the generator cylinder and used for conveying phosphorus pentafluoride gas to a next process device,
the upper cylinder is provided with liquid material feeders for feeding liquid hydrogen fluoride into the generator cylinder, and each liquid material feeder is connected with the liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline;
the lower cylinder is provided with a liquid hydrogen fluoride permeation jacket arranged along the inner wall of the lower cylinder, the liquid hydrogen fluoride permeation jacket is provided with an isolation filter plate used for bearing and contacting the phosphorus pentachloride solid material in the generator cylinder, and the liquid hydrogen fluoride permeation jacket is connected with a liquid hydrogen fluoride supply device through a liquid hydrogen fluoride supply pipeline;
the liquid hydrogen fluoride supplied to the liquid hydrogen fluoride permeation jacket by the liquid hydrogen fluoride supply device permeates into the generator cylinder through the isolation filter plate and reacts with the phosphorus pentachloride solid material in the generator cylinder.
2. The phosphorus pentafluoride gas generator of claim 1,
the liquid hydrogen fluoride permeating jacket is at least formed by the isolation filter plate in a cone shape.
3. The phosphorus pentafluoride gas generator of claim 1 or 2,
the isolation filter plate adopts a plurality of layers of sintered filter screens.
4. The phosphorus pentafluoride gas generator of claim 1 or 2,
and a cooling jacket is arranged on the outer wall of at least one of the upper cylinder and the lower cylinder and is connected with a cooling circulation device through a cooling medium conveying pipeline.
5. The phosphorus pentafluoride gas generator of claim 1 or 2,
the stirring device is provided with a spiral belt with a hollow structure, and the spiral belt is connected with the cooling circulation device.
6. The phosphorus pentafluoride gas generator of claim 1 or 2,
and a powder filter is arranged on the gas conveying pipeline.
7. The phosphorus pentafluoride gas generator of claim 4,
a temperature transmitter is arranged in the generator cylinder, and a regulating valve is arranged on the cooling medium conveying pipeline.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222001109.XU CN218088970U (en) | 2022-08-01 | 2022-08-01 | Phosphorus pentafluoride gas generator |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202222001109.XU CN218088970U (en) | 2022-08-01 | 2022-08-01 | Phosphorus pentafluoride gas generator |
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| Publication Number | Publication Date |
|---|---|
| CN218088970U true CN218088970U (en) | 2022-12-20 |
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN202222001109.XU Withdrawn - After Issue CN218088970U (en) | 2022-08-01 | 2022-08-01 | Phosphorus pentafluoride gas generator |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115072681A (en) * | 2022-08-01 | 2022-09-20 | 森松（江苏）重工有限公司 | Phosphorus pentafluoride gas generator and phosphorus pentafluoride gas generating method |
-
2022
- 2022-08-01 CN CN202222001109.XU patent/CN218088970U/en not_active Withdrawn - After Issue
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115072681A (en) * | 2022-08-01 | 2022-09-20 | 森松（江苏）重工有限公司 | Phosphorus pentafluoride gas generator and phosphorus pentafluoride gas generating method |
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Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| GR01 | Patent grant | ||
| GR01 | Patent grant | ||
| CB03 | Change of inventor or designer information | ||
| CB03 | Change of inventor or designer information |
Inventor after: Li Zhenxing Inventor after: Xu Cheng Inventor after: Chen Hongwei Inventor after: Nishimatsu Kohide Inventor before: Li Zhenxing Inventor before: Xu Cheng Inventor before: Chen Hongwei |
|
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned | ||
| AV01 | Patent right actively abandoned |
Granted publication date: 20221220 Effective date of abandoning: 20230714 |
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| AV01 | Patent right actively abandoned |
Granted publication date: 20221220 Effective date of abandoning: 20230714 |