CN219072522U - Energy-saving type lithium hexafluorophosphate production tail gas deep-cooling efficient separation and purification device - Google Patents
Energy-saving type lithium hexafluorophosphate production tail gas deep-cooling efficient separation and purification device Download PDFInfo
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- CN219072522U CN219072522U CN202223613164.0U CN202223613164U CN219072522U CN 219072522 U CN219072522 U CN 219072522U CN 202223613164 U CN202223613164 U CN 202223613164U CN 219072522 U CN219072522 U CN 219072522U
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Abstract
The utility model discloses a deep cooling high-efficiency separation and purification device for energy-saving lithium hexafluorophosphate production tail gas, which comprises a precooler, an intercooler, a deep cooler, a hydrogen fluoride recovery pipeline and a hydrochloric acid recovery pipeline, wherein the lithium hexafluorophosphate production tail gas sequentially passes through the precooler, the intercooler and the deep cooler; the precooler and the cryocooler are both communicated with the hydrogen fluoride recovery pipeline, and the intercooler is communicated with the hydrochloric acid recovery pipeline; the cold source of the intercooler is liquid nitrogen, the cold source of the precooler is low-temperature nitrogen exhausted by the intercooler, and the cold source of the intercooler is low-temperature non-condensable gas exhausted by the intercooler. The device can efficiently separate HF and HCl components in tail gas generated in lithium hexafluorophosphate production, and saves energy.
Description
Technical Field
The utility model relates to the technical field of tail gas recovery equipment, in particular to a deep-cooling high-efficiency separation and purification device for tail gas in lithium hexafluorophosphate production.
Background
At present, a wet process is generally adopted to produce lithium hexafluorophosphate, and PCl is firstly adopted in the production step 5 Reaction with anhydrous HF to produce PF 5 Then reacts with LiF dissolved in HF solution to generate LiPF 6 The overall reaction is carried out in anhydrous HF solution, with HF being both the reaction precursor and the solvent, and must be used in excess. In the production process of lithium hexafluorophosphate, a great deal of HF volatilizes due to severe reaction in the feeding reaction process, and the HF volatilizes together with byproduct HCl from a reaction kettle to form lithium hexafluorophosphate production tail gas.
The conventional tail gas treatment process at present is to set a-30 ℃ condensing reflux part of HF at the discharge outlet of a reaction kettle, and then spray and absorb the uncondensed HF and HCl by water to obtain mixed acid liquid. The key problem of the tail gas treatment process is that the condensing efficiency at the temperature of minus 30 ℃ is low, HF cannot be recovered efficiently, a great amount of HF is wasted, only mixed waste liquid of HF and HCl can be obtained, and the waste liquid is required to be treated.
Disclosure of Invention
The utility model aims to provide an energy-saving cryogenic high-efficiency separation and purification device for lithium hexafluorophosphate production tail gas, which can efficiently separate HF and HCl components in the lithium hexafluorophosphate production tail gas and save energy.
To achieve the purpose, the utility model adopts the following technical scheme:
the energy-saving type lithium hexafluorophosphate production tail gas deep-cooling high-efficiency separation and purification device comprises a precooler, an intercooler, a cryocooler, a hydrogen fluoride recovery pipeline and a hydrochloric acid recovery pipeline, wherein the lithium hexafluorophosphate production tail gas sequentially passes through the precooler, the intercooler and the cryocooler;
the precooler and the cryocooler are both communicated with the hydrogen fluoride recovery pipeline, and the intercooler is communicated with the hydrochloric acid recovery pipeline;
the cold source of the intercooler is liquid nitrogen, the cold source of the precooler is low-temperature nitrogen exhausted by the intercooler, and the cold source of the intercooler is low-temperature non-condensable gas exhausted by the intercooler.
Further, the upper part of the precooler is communicated with the upper part of the cryocooler through a first cold source pipeline, and the first cold source pipeline is used for guiding low-temperature nitrogen discharged by the cryocooler into the precooler;
and the top of the precooler is connected with a tail gas feeding pipeline.
Further, the lower part of the precooler is communicated with a nitrogen recycling device, and the nitrogen recycling device is used for collecting nitrogen discharged from the precooler.
Further, the upper part of the intercooler is communicated with the top of the intercooler through a second cold source pipeline, and the second cold source pipeline is used for guiding low-temperature non-condensable gas exhausted by the intercooler into the intercooler.
Further, the lower part of the precooler is communicated with the lower part of the intercooler through a first discharging pipeline, and the first discharging pipeline is used for guiding the tail gas treated by the precooler into the intercooler.
Further, the top of intercooler is linked together through second ejection of compact pipeline with the lower part of intercooler, second ejection of compact pipeline is used for will be passed through the tail gas of intercooler treatment is directed into the intercooler, the lower part of intercooler is connected with the liquid nitrogen pipe.
Further, the liquid nitrogen pipe is provided with a liquid nitrogen regulating valve;
and a temperature sensor is arranged at one end of the second discharging pipeline, which is close to the refrigerator, and the liquid nitrogen regulating valve is electrically connected with the temperature sensor.
Further, the bottom of the precooler and the bottom of the cryocooler are respectively communicated with the hydrogen fluoride recovery pipeline;
the tail end of the hydrogen fluoride recovery pipeline is provided with a hydrogen fluoride temporary storage tank.
Further, one end of the hydrochloric acid recovery pipeline is communicated with the bottom of the intercooler, and a first recovery branch and a second recovery branch are arranged at the other end of the hydrochloric acid recovery pipeline;
the first recovery branch is provided with a hydrochloric acid falling film absorption device, and the second recovery branch is provided with an active alumina purification device.
The technical scheme provided by the utility model can comprise the following beneficial effects:
the utility model is provided with the precooler, the intercooler and the cryocooler, adopts a multistage cryogenic condensation mode, can efficiently separate HF and HCl components in lithium hexafluorophosphate production tail gas, HF can be recycled to a production flow, the separated HCl gas has high purity, and the HCl gas can be absorbed by a hydrochloric acid falling film to generate industrial grade hydrochloric acid with the purity of 99.9 percent, or is purified by activated alumina to obtain high purity HCl gas with the purity of 5N.
In the utility model, the cold source of the precooler is low-temperature nitrogen discharged by the cryogenic refrigerator, and the cold source of the intercooler is low-temperature non-condensable gas discharged by the cryogenic refrigerator, so that the utilization rate of liquid nitrogen can be fully improved, and the energy-saving effect is achieved.
Drawings
FIG. 1 is a schematic diagram of a cryogenic efficient separation/purification apparatus according to an embodiment of the utility model;
the device comprises a precooler 10, an intercooler 20, a cryocooler 30, a nitrogen recycling device 40, a hydrogen fluoride recovery pipeline 1, a hydrogen fluoride temporary storage tank 11, a hydrochloric acid recovery pipeline 2, a first recovery branch 21, a hydrochloric acid falling film absorption device 23, a second recovery branch 22, an activated alumina purification device 24, a first cold source pipeline 3, a second cold source pipeline 4, a first discharge pipeline 5, a second discharge pipeline 6, a temperature sensor 61, a liquid nitrogen pipe 7 and a liquid nitrogen regulating valve 71.
Detailed Description
Embodiments of the present utility model are described in detail below, examples of which are illustrated in the accompanying drawings, wherein like or similar reference numerals refer to like or similar elements or elements having like or similar functions throughout. The embodiments described below by referring to the drawings are illustrative only and are not to be construed as limiting the utility model.
In the description of the present utility model, it should be understood that the directions or positional relationships indicated by the terms "upper", "lower", "top", "bottom", etc. are based on the directions or positional relationships shown in the drawings, are merely for convenience of description and simplification of the description, and do not indicate or imply that the apparatus or element in question must have a specific orientation, be constructed and operated in a specific orientation, and therefore should not be construed as limiting the utility model. Furthermore, features defining "first", "second" may include one or more such features, either explicitly or implicitly, for distinguishing between the descriptive features, and not sequentially, and not lightly.
In the description of the present utility model, it should be noted that, unless explicitly specified and limited otherwise, the terms "mounted," "connected," and "connected" are to be construed broadly, and may be either fixedly connected, detachably connected, or integrally connected, for example; can be mechanically or electrically connected; can be directly connected or indirectly connected through an intermediate medium, and can be communication between two elements. The specific meaning of the above terms in the present utility model will be understood in specific cases by those of ordinary skill in the art.
The following describes a cryogenic high-efficiency separation and purification device for tail gas generated in the production of energy-saving lithium hexafluorophosphate according to an embodiment of the utility model with reference to fig. 1.
The energy-saving type lithium hexafluorophosphate production tail gas deep-cooling high-efficiency separation and purification device comprises a precooler 10, an intercooler 20, a cryocooler 30, a hydrogen fluoride recovery pipeline 1 and a hydrochloric acid recovery pipeline 2, wherein the lithium hexafluorophosphate production tail gas sequentially passes through the precooler 10, the intercooler 20 and the cryocooler 30;
the precooler 10 and the cryocooler 30 are both communicated with a hydrogen fluoride recovery pipeline 1, and the intercooler 20 is communicated with a hydrochloric acid recovery pipeline 2;
the cold source of the cryocooler 30 is liquid nitrogen, the cold source of the precooler 10 is low-temperature nitrogen discharged by the cryocooler 30, and the cold source of the intercooler 20 is low-temperature non-condensable gas discharged by the cryocooler 30.
The precooler 10, the intercooler 20 and the cryocooler 30 are arranged, a multistage cryocondensation mode is adopted, HF and HCl components in lithium hexafluorophosphate production tail gas can be efficiently separated, the purity of recovered HF condensate is 98.3%, the recovery rate is over 99.9%, HF can be recycled to a production flow, and the production cost of lithium hexafluorophosphate is reduced to a great extent; the purity of the HCl gas obtained by separation is high, and economic benefit is generated.
In the utility model, the cold source of the precooler 10 is low-temperature nitrogen discharged by the cryocooler 30, and the cold source of the intercooler 20 is low-temperature non-condensable gas discharged by the cryocooler 30, so that the utilization rate of liquid nitrogen can be fully improved, and the energy-saving effect can be achieved.
Specifically, the process of treating tail gas from lithium hexafluorophosphate production by using the cryogenic high-efficiency separation and purification device comprises the following steps: the tail gas firstly enters the precooler 10, most HF in the tail gas is condensed into the hydrogen fluoride recovery pipeline 1 under the cooling effect of low-temperature nitrogen discharged by the cryocooler 30, noncondensable gas in the precooler 10 enters the intercooler 20, the low-temperature noncondensable gas discharged by the cryocooler 30 in the intercooler 20 is continuously cooled, most HCl gas in the tail gas enters the hydrochloric acid recovery pipeline 2, noncondensable gas in the intercooler 20 enters the cryocooler 30, and the residual HF in the tail gas is condensed again and enters the hydrogen fluoride recovery pipeline 1.
Further, the upper part of the precooler 10 is communicated with the upper part of the cryocooler 30 through a first cold source pipeline 3, and the first cold source pipeline 3 is used for guiding low-temperature nitrogen discharged by the cryocooler 30 into the precooler 10; the top of the precooler 10 is connected with a tail gas feed pipe. The tail gas from lithium hexafluorophosphate production enters the precooler 10 from the tail gas feeding pipeline, and the tail gas and the low-temperature nitrogen gas move from the top to the bottom of the precooler 10 together, so that the cold energy of the low-temperature nitrogen gas can be fully utilized.
Further, the lower part of the precooler 10 is communicated with a nitrogen recycling device 40, the nitrogen recycling device 40 is used for collecting nitrogen discharged from the precooler 10, the recycled nitrogen is recycled to a nitrogen pipe network of a workshop after the temperature of the nitrogen is increased to be close to the outdoor temperature by the nitrogen recycling device 40 and the pressure is adjusted, and the nitrogen recycling device is used for processes such as nitrogen pressure material, nitrogen replacement, nitrogen purging, nitrogen sealing and the like.
Further, the upper portion of the intercooler 20 is communicated with the top of the intercooler 30 through a second cold source duct 4, and the second cold source duct 4 is used for guiding the low-temperature non-condensable gas discharged from the intercooler 30 into the intercooler 20. In addition, the lower part of the precooler 10 is communicated with the lower part of the intercooler 20 through a first discharging pipeline 5, and the first discharging pipeline 5 is used for guiding the tail gas treated by the precooler 10 into the intercooler 20. In the intercooler 20, the tail gas upwards moves from the lower part of the intercooler 20, the low-temperature non-condensable gas exhausted by the intercooler 30 moves from the upper part of the intercooler 20 to the lower part, and the tail gas and the low-temperature non-condensable gas move in opposite directions, so that the effect of fully cooling the tail gas is achieved, and the recovery rate of HCl is further improved.
Further, the top of the intercooler 20 is communicated with the lower part of the cryocooler 30 through a second discharging pipeline 6, the second discharging pipeline 6 is used for guiding the tail gas treated by the intercooler 20 into the cryocooler 30, and the lower part of the cryocooler 30 is connected with a liquid nitrogen pipe 7. In the cryocooler 30, the liquid nitrogen and the tail gas from the intercooler 20 move from the lower part to the upper part of the cryocooler 30, the heat exchange time of the two mediums is long, the HF gas in the tail gas can be fully condensed, and the recovery efficiency is improved. Specifically, liquid nitrogen is supplied to the cryogenic refrigerator 30 through the liquid nitrogen pipe 7 by pressure in the liquid nitrogen tank.
Further, the liquid nitrogen pipe 7 is provided with a liquid nitrogen regulating valve 71, and the flow of liquid nitrogen is controlled through the liquid nitrogen regulating valve 71, so that the condensation temperature of the cryogenic condenser is controllable; the second discharge pipe 6 is provided with a temperature sensor 61 at one end close to the refrigerator 30, and a liquid nitrogen regulating valve 71 is electrically coupled to the temperature sensor 61. The temperature sensor 61 is used to sense the feed temperature of the chiller 30. In actual production, the feeding temperature of the chiller 30 is preset, when the temperature sensed by the temperature sensor 61 is greater than the set temperature, the liquid nitrogen regulating valve 71 increases the opening, and when the temperature sensed by the temperature sensor 61 is less than the set temperature, the liquid nitrogen regulating valve 71 decreases the opening, so that the cryogenic condensing temperature as low as-160 ℃ can be realized.
Further, the bottom of the precooler 10 and the bottom of the cryocooler 30 are respectively communicated with a hydrogen fluoride recovery pipeline 1; the tail end of the hydrogen fluoride recovery pipeline 1 is provided with a hydrogen fluoride temporary storage tank 11. The discharge pipeline of the hydrogen fluoride temporary storage tank 11 is provided with a delivery pump for pumping the hydrogen fluoride back to the lithium hexafluorophosphate production line.
Further, one end of the hydrochloric acid recovery pipeline 2 is communicated with the bottom of the intercooler 20, and a first recovery branch 21 and a second recovery branch 22 are arranged at the other end of the hydrochloric acid recovery pipeline 2; the first recovery branch 21 is provided with a hydrochloric acid falling film absorption device 23, and the second recovery branch 22 is provided with an activated alumina purification device 24. The HCl gas can be absorbed by hydrochloric acid falling film to produce industrial grade hydrochloric acid with purity of 99.9 percent, or purified by activated alumina to obtain high-purity HCl gas with purity of 5N. Specifically, the first recovery branch 21 and the second recovery branch 22 are both provided with valves, and industrial grade hydrochloric acid or high-purity HCl gas can be produced by using HCl gas through selectively opening the valves.
Other components and operations of a cryogenic high-efficiency separation and purification device for tail gas from lithium hexafluorophosphate production according to embodiments of the present utility model are known to those skilled in the art, and will not be described in detail herein.
In the description herein, reference to the term "embodiment," "example," etc., means that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the utility model. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
While embodiments of the present utility model have been shown and described, it will be understood by those of ordinary skill in the art that: many changes, modifications, substitutions and variations may be made to the embodiments without departing from the spirit and principles of the utility model, the scope of which is defined by the claims and their equivalents.
Claims (9)
1. The energy-saving type lithium hexafluorophosphate production tail gas deep-cooling high-efficiency separation and purification device is characterized by comprising a precooler, an intercooler, a deep cooler, a hydrogen fluoride recovery pipeline and a hydrochloric acid recovery pipeline, wherein the lithium hexafluorophosphate production tail gas sequentially passes through the precooler, the intercooler and the deep cooler;
the precooler and the cryocooler are both communicated with the hydrogen fluoride recovery pipeline, and the intercooler is communicated with the hydrochloric acid recovery pipeline;
the cold source of the intercooler is liquid nitrogen, the cold source of the precooler is low-temperature nitrogen exhausted by the intercooler, and the cold source of the intercooler is low-temperature non-condensable gas exhausted by the intercooler.
2. The apparatus of claim 1, wherein an upper portion of the precooler is in communication with an upper portion of the cryogenic refrigerator through a first cold source conduit for introducing cryogenic nitrogen discharged from the cryogenic refrigerator into the precooler;
and the top of the precooler is connected with a tail gas feeding pipeline.
3. The apparatus of claim 2, wherein a nitrogen reclamation apparatus is in communication with a lower portion of the precooler, the nitrogen reclamation apparatus being configured to collect nitrogen discharged from the precooler.
4. The apparatus of claim 1, wherein an upper portion of the intercooler is in communication with a top portion of the intercooler through a second cold source conduit for introducing low temperature non-condensable gases exiting the intercooler into the intercooler.
5. The apparatus of claim 1, wherein a lower portion of the precooler is in communication with a lower portion of the intercooler via a first discharge conduit for directing tail gas treated by the precooler to the intercooler.
6. The apparatus of claim 5, wherein the top of the intercooler is in communication with a lower portion of the intercooler via a second discharge conduit for introducing tail gas treated by the intercooler into the intercooler, the lower portion of the intercooler being connected to a liquid nitrogen pipe.
7. The device according to claim 6, wherein the liquid nitrogen pipe is provided with a liquid nitrogen regulating valve;
and a temperature sensor is arranged at one end of the second discharging pipeline, which is close to the refrigerator, and the liquid nitrogen regulating valve is electrically connected with the temperature sensor.
8. The apparatus of claim 1, wherein a bottom of the pre-cooler and a bottom of the cryocooler are each in communication with the hydrogen fluoride recovery conduit;
the tail end of the hydrogen fluoride recovery pipeline is provided with a hydrogen fluoride temporary storage tank.
9. The apparatus of claim 1, wherein one end of the hydrochloric acid recovery pipe is communicated with the bottom of the intercooler, and the other end of the hydrochloric acid recovery pipe is provided with a first recovery branch and a second recovery branch;
the first recovery branch is provided with a hydrochloric acid falling film absorption device, and the second recovery branch is provided with an active alumina purification device.
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| CN202223613164.0U CN219072522U (en) | 2022-12-30 | 2022-12-30 | Energy-saving type lithium hexafluorophosphate production tail gas deep-cooling efficient separation and purification device |
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| CN202223613164.0U CN219072522U (en) | 2022-12-30 | 2022-12-30 | Energy-saving type lithium hexafluorophosphate production tail gas deep-cooling efficient separation and purification device |
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