CN216236054U - Lithium hexafluorophosphate continuous method synthesis system - Google Patents
Lithium hexafluorophosphate continuous method synthesis system Download PDFInfo
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Abstract
The utility model relates to a lithium hexafluorophosphate continuous synthesis system, which comprises a first micro-pipeline reactor, a first gas-liquid separator, a purification device and a second micro-pipeline reactor, wherein the first micro-pipeline reactor is connected with the first gas-liquid separator through a pipeline; a liquid inlet of the first micro-pipeline reactor is respectively connected with liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid; the reaction liquid outlet of the first micro-pipeline reactor is connected with the inlet of the first gas-liquid separator, the gas outlet of the first gas-liquid separator is connected with the purifying device, and the liquid outlet of the purifying device is connected with the second micro-pipeline reactor. Under the production of continuously synthesizing lithium hexafluorophosphate, reaction steps can be saved, the control of reaction conditions is reduced, the energy consumption is reduced, the operation is reduced, and the purity of reaction products can be ensured.
Description
Technical Field
The utility model belongs to the technical field of preparation of lithium hexafluorophosphate, and particularly relates to a lithium hexafluorophosphate continuous method synthesis system.
Background
The information in this background section is only for enhancement of understanding of the general background of the utility model and is not necessarily to be construed as an admission or any form of suggestion that this information forms the prior art that is already known to a person of ordinary skill in the art.
In the existing preparation process of lithium hexafluorophosphate, hydrogen fluoride and sulfur trioxide are required to react to obtain fluorosulfonic acid, then the fluorosulfonic acid reacts with polyphosphoric acid to obtain phosphorus pentafluoride, and then the reaction is carried out to obtain lithium hexafluorophosphate. And the obtained lithium hexafluorophosphate has high impurity content, which affects the purity of the lithium hexafluorophosphate.
SUMMERY OF THE UTILITY MODEL
In view of the problems in the prior art, the utility model aims to provide a lithium hexafluorophosphate continuous method synthesis system.
In order to solve the technical problems, the technical scheme of the utility model is as follows:
a lithium hexafluorophosphate continuous method synthesis system comprises a first micro-pipeline reactor, a first gas-liquid separator, a purification device and a second micro-pipeline reactor; a liquid inlet of the first micro-pipeline reactor is respectively connected with liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid; the reaction liquid outlet of the first micro-pipeline reactor is connected with the inlet of the first gas-liquid separator, the gas outlet of the first gas-liquid separator is connected with the purifying device, and the liquid outlet of the purifying device is connected with the second micro-pipeline reactor.
According to the lithium hexafluorophosphate synthesis system provided by the utility model, sulfur trioxide, hydrogen fluoride and polyphosphoric acid react together to obtain gaseous phosphorus pentafluoride and sulfuric acid, and after gas-liquid separation, the gaseous phosphorus pentafluoride is purified and then enters a second micro-pipeline reactor to react to obtain phosphorus hexafluoride. The reaction equation is as follows:
13SO3+20HF+H6P4O13→4PF5+13H2S04
the sulfur trioxide, the hydrogen fluoride and the polyphosphoric acid are reacted simultaneously, the problem that the hydrogen fluoride and the sulfur trioxide react to obtain the fluorosulfonic acid first is solved, then the fluorosulfonic acid and the polyphosphoric acid react to obtain the phosphorus pentafluoride is solved, and the reaction process is reduced.
Then the gaseous phosphorus pentafluoride enters a purification device to remove sulfur trioxide and hydrogen fluoride substances carried in the phosphorus pentafluoride, and the purer phosphorus pentafluoride is obtained. The purity of lithium hexafluorophosphate obtained by the reaction of phosphorus pentafluoride in the next step is improved.
One or more technical schemes of the utility model have the following beneficial effects:
according to the lithium hexafluorophosphate continuous synthesis system provided by the utility model, the three substances of sulfur trioxide, hydrogen fluoride and polyphosphoric acid are added at the same time through the micro-pipeline reactor and react, so that the reaction steps are reduced, the gas phosphorus pentafluoride can be directly obtained, and the reaction process of lithium hexafluorophosphate can be directly carried out after purification by the purification device. The whole process can be continuously carried out, reaction steps can be saved, the control of reaction conditions is reduced, the energy consumption is reduced, the operation is reduced, and the purity of reaction products can be ensured under the production of continuously synthesizing lithium hexafluorophosphate.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the utility model, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the utility model and together with the description serve to explain the utility model and not to limit the utility model.
FIG. 1 is a schematic diagram of a lithium hexafluorophosphate continuous process synthesis system;
the device comprises a first micro-pipeline reactor 1, a first gas-liquid separator 2, a first gas-liquid separator 3, an acid mixing tank 4, a gas-liquid mixer 5, a second gas-liquid separator 6, a second micro-pipeline reactor 7, a third gas-liquid separator 8, a filter 9, a micro-crystallizer 10, a dryer 11, a third micro-pipeline reactor 12, a dissolving tank 13, an HF source 14, fuming sulfuric acid 15, polyphosphoric acid 16, an LiF source 17, a nitrogen source 18, a product 19 and tail gas.
Detailed Description
It is to be understood that the following detailed description is exemplary and is intended to provide further explanation of the utility model as claimed. Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this disclosure belongs.
It is noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of example embodiments according to the present disclosure. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
A lithium hexafluorophosphate continuous method synthesis system comprises a first micro-pipeline reactor 1, a first gas-liquid separator 2, a purification device and a second micro-pipeline reactor 6; a liquid inlet of the first micro-pipeline reactor 1 is respectively connected with liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid; the reaction liquid outlet of the first micro-pipeline reactor is connected with the inlet of the first gas-liquid separator 2, the gas outlet of the first gas-liquid separator 2 is connected with the purifying device, and the liquid outlet of the purifying device is connected with the second micro-pipeline reactor 6.
According to the lithium hexafluorophosphate synthesis system provided by the utility model, sulfur trioxide, hydrogen fluoride and polyphosphoric acid react together to obtain gaseous phosphorus pentafluoride and sulfuric acid, and after gas-liquid separation, the gaseous phosphorus pentafluoride is purified and then enters a second micro-pipeline reactor to react to obtain phosphorus hexafluoride. The reaction equation is as follows:
13SO3+20HF+H6P4O13→4PF5+13H2S04
oleum is introduced to generate sulfur trioxide.
And the gas phosphorus pentafluoride generated by the first micro-pipeline reactor enters a purification device to remove impurities such as sulfur trioxide carried in the gas phosphorus pentafluoride. The whole process can omit the reaction step, and the purity of the lithium hexafluorophosphate product can be improved after purification,
As a further technical scheme, the purification device is a gas-liquid mixer 4, and the gas-liquid mixer 4 is connected with a hydrogen fluoride source. The purification device utilizes hydrogen fluoride to dissolve phosphorus pentafluoride, the phosphorus pentafluoride is easily dissolved in liquid hydrogen fluoride (HF is liquid at normal temperature under certain pressure) to obtain a liquid mixture, then the liquid mixture enters the second gas-liquid separator to separate the carried liquid hydrogen fluoride, and then the gas of the obtained phosphorus pentafluoride enters the second micro-pipeline reactor to react. The pressure may be 8kg/cm2。
The reaction carried out in the second microchannel reactor is as follows:
PF5+LiF+HF→LiPF6+HF。
as a further technical scheme, the purification device further comprises a second gas-liquid separator 5, a liquid outlet of the gas-liquid mixer 4 is connected with the second gas-liquid separator 5, and a gas outlet of the second gas-liquid separator is connected with the second micro-pipeline reactor.
As a further technical solution, the liquid outlet of the second gas-liquid separator 5 is connected to a hydrogen fluoride source. The liquid discharged from the liquid outlet is mainly a hydrogen fluoride liquid substance.
As a further technical scheme, liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid are respectively connected with the first micro-pipeline reactor, and liquid inlet pumps are respectively arranged on the liquid inlet pipelines. The HF source 13, the polyphosphoric acid source 15 and the oleum source 14 enter the first microchannel reactor 1 respectively.
As a further technical scheme, the device also comprises an acid mixing tank 3, and the liquid outlet of the first gas-liquid separator 2 is connected with the liquid inlet of the acid mixing tank 3. The liquid discharged from the acid mixing tank comprises polyphosphoric acid and sulfuric acid.
As a further technical scheme, the device also comprises a third gas-liquid separator 7, and the gas outlet of the second micro-pipeline reactor 6 is connected with the third gas-liquid separator 7. And the lithium hexafluorophosphate and the hydrogen fluoride gas obtained by the second micro-pipeline reactor 6 enter a gas-liquid separator for separation to obtain gaseous hydrogen fluoride and liquid lithium hexafluorophosphate, and the gaseous hydrogen fluoride enters a third micro-pipeline reactor 7.
As a further technical scheme, the device also comprises a third micro-pipeline reactor 11, and the air outlet of the third gas-liquid separator 7 is connected with the third micro-pipeline reactor 11.
As a further technical scheme, the device further comprises a dissolving tank 12, wherein the dissolving tank 12 is connected with a third micro-pipeline reactor 11, the dissolving tank 12 is respectively connected with a hydrogen fluoride source 13 and a lithium fluoride source 16, and a liquid outlet of the third micro-pipeline reactor. The third pipeline reactor is used for fully mixing and absorbing the mixture of the lithium fluoride and the hydrogen fluoride entering the third pipeline reactor with the third gas-liquid separator, and the mixed liquid obtained after absorption enters the second micro-pipeline reactor to be used as a raw material to participate in the reaction. Lithium fluoride is dissolved in hydrogen fluoride liquid under a certain pressure.
As a further technical scheme, the device also comprises a filter 8, a micro-crystallizer 9 and a dryer 10, wherein the liquid outlet of the third gas-liquid separator 7 is connected with the filter 8, the micro-crystallizer 9 and the dryer 10 in sequence. Further, the dryer 10 is connected to a nitrogen gas source 17. The dryer 10 produces a tail gas 19 and the dryer 10 produces a final lithium hexafluorophosphate product 18. The mother liquor produced by the micro-crystallizer 9 is recycled to the dissolving tank 12.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. A lithium hexafluorophosphate continuous method synthesis system is characterized in that: comprises a first micro-pipeline reactor, a first gas-liquid separator, a purification device and a second micro-pipeline reactor; a liquid inlet of the first micro-pipeline reactor is respectively connected with liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid; the reaction liquid outlet of the first micro-pipeline reactor is connected with the inlet of the first gas-liquid separator, the gas outlet of the first gas-liquid separator is connected with the purifying device, and the liquid outlet of the purifying device is connected with the second micro-pipeline reactor.
2. The lithium hexafluorophosphate continuous process synthesis system of claim 1, wherein: the purification device is a gas-liquid mixer, and the gas-liquid mixer is connected with the hydrogen fluoride source.
3. The lithium hexafluorophosphate continuous process synthesis system of claim 2, wherein: the purification device also comprises a second gas-liquid separator, a liquid outlet of the gas-liquid mixer is connected with the second gas-liquid separator, and a gas outlet of the second gas-liquid separator is connected with the second micro-pipeline reactor.
4. A lithium hexafluorophosphate continuous process synthesis system according to claim 3, wherein: the liquid outlet of the second gas-liquid separator is connected with a hydrogen fluoride source.
5. The lithium hexafluorophosphate continuous process synthesis system of claim 1, wherein: the liquid inlet pipelines of sulfur trioxide, hydrogen fluoride and polyphosphoric acid are respectively connected with the first micro-pipeline reactor, and a liquid inlet pump is respectively arranged on each liquid inlet pipeline.
6. The lithium hexafluorophosphate continuous process synthesis system of claim 1, wherein: the device also comprises an acid mixing tank, wherein the liquid outlet of the first gas-liquid separator is connected with the liquid inlet of the acid mixing tank.
7. The lithium hexafluorophosphate continuous process synthesis system of claim 1, wherein: the gas outlet of the second micro-pipeline reactor is connected with the third gas-liquid separator.
8. The lithium hexafluorophosphate continuous process synthesis system of claim 7, wherein: the gas outlet of the third gas-liquid separator is connected with the third micro-pipeline reactor.
9. The lithium hexafluorophosphate continuous process synthesis system of claim 8, wherein: the device also comprises a dissolving tank, wherein the dissolving tank is connected with the third micro-pipeline reactor, the dissolving tank is respectively connected with a hydrogen fluoride source and a lithium fluoride source, and a liquid outlet of the third micro-pipeline reactor.
10. The lithium hexafluorophosphate continuous process synthesis system of claim 7, wherein: the liquid outlet of the third gas-liquid separator is connected with the filter, the micro-crystallizer and the dryer in sequence.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN117504763A (en) * | 2023-11-09 | 2024-02-06 | 多氟多海纳新材料有限责任公司 | Lithium hexafluorophosphate production system based on microchannel reactor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117504763A (en) * | 2023-11-09 | 2024-02-06 | 多氟多海纳新材料有限责任公司 | Lithium hexafluorophosphate production system based on microchannel reactor |
| CN117504763B (en) * | 2023-11-09 | 2024-07-30 | 多氟多海纳新材料有限责任公司 | Lithium hexafluorophosphate production system based on microchannel reactor |
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