CN105731413A - Phosphorus pentafluoride reaction still, phosphorus pentafluoride and preparation method for lithium hexafluorophosphate - Google Patents
Phosphorus pentafluoride reaction still, phosphorus pentafluoride and preparation method for lithium hexafluorophosphate Download PDFInfo
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- CN105731413A CN105731413A CN201610235238.1A CN201610235238A CN105731413A CN 105731413 A CN105731413 A CN 105731413A CN 201610235238 A CN201610235238 A CN 201610235238A CN 105731413 A CN105731413 A CN 105731413A
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- phosphorus pentafluoride
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- acid gas
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- fluohydric acid
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01D—COMPOUNDS OF ALKALI METALS, i.e. LITHIUM, SODIUM, POTASSIUM, RUBIDIUM, CAESIUM, OR FRANCIUM
- C01D15/00—Lithium compounds
- C01D15/005—Lithium hexafluorophosphate
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/10—Halides or oxyhalides of phosphorus
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- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
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Abstract
The invention discloses a phosphorus pentafluoride reaction still, phosphorus pentafluoride and a preparation method for lithium hexafluorophosphate.The phosphorus pentafluoride reaction still comprises a reaction still body and a hydrogen fluoride pipeline communicated with the reaction still body.A heating device is arranged on the hydrogen fluoride pipeline.Through the heating device, hydrogen fluoride in the hydrogen fluoride pipeline is always in a gasified state, gas-state hydrogen fluoride reacts with phosphorus pentachloride, the intensity is reduced, and product quality is high.
Description
Technical field
The application belongs to electrode of lithium cell raw material field, particularly relates to a kind of phosphorus pentafluoride reactor, phosphorus pentafluoride and lithium hexafluoro phosphate preparation method.
Background technology
Lithium hexafluoro phosphate is as the important electrolytic salt of lithium-ion battery electrolytes, it is desirable to it has significantly high purity (generally otherwise lower than 99.5%), impurity therein such as moisture content, alkali metal, heavy metal and other impurity such as PCl3And POCl3Content must strictly control, otherwise will cause that the internal resistance of cell increases, battery capacity decay is fast, and cycle life shortens, and even affects the safety of battery.The lithium hexafluoro phosphate product of the objectionable impurities obtaining high-purity and low content is significant.
In traditional lithium hexafluoro phosphate preparation process, fluohydric acid gas is generally fed in reactor with liquid, and there is fluohydric acid gas with liquid and react acutely with phosphorus pentachloride, affects product quality.
Summary of the invention
It is an object of the invention to provide a kind of phosphorus pentafluoride reactor, phosphorus pentafluoride and lithium hexafluoro phosphate preparation method, to overcome deficiency of the prior art.
For achieving the above object, the present invention provides following technical scheme:
The open a kind of phosphorus pentafluoride reactor of the embodiment of the present application, including reactor and the fluohydric acid gas pipeline that connects with reactor, described fluohydric acid gas pipeline is provided with heater.
Preferably, in above-mentioned phosphorus pentafluoride reactor, described heater is be set around electrical heating wire on described fluohydric acid gas pipeline or water circulation pipe.
Preferably, in above-mentioned phosphorus pentafluoride reactor, described heater to fluohydric acid gas pipeline heating so that its temperature is more than hydrofluoric gasification temperature.
Preferably, in above-mentioned phosphorus pentafluoride reactor, described heater includes:
Temperature sensor, the in real time temperature in detection fluohydric acid gas pipeline, and this temperature information is sent to controller；
Controller, processes temperature information, and fluohydric acid gas pipeline is heated, and is positioned between setting district controlling temperature in pipeline.
Accordingly, the preparation method that disclosed herein as well is a kind of phosphorus pentafluoride, including:
(1), phosphorus pentachloride is put in reactor；
(2), passing in reactor by the fluohydric acid gas after gasification, reaction obtains phosphorus pentafluoride.
Preferably, in the preparation method of above-mentioned phosphorus pentafluoride, in described step (2), reaction temperature is 178～182 DEG C, and reaction pressure is 0.13～0.17MPa.
The preparation method that disclosed herein as well is a kind of lithium hexafluoro phosphate, comprises the steps:
(1), hydrogen fluoride gas is passed in the reactor adding phosphorus pentachloride, temperature is controlled between 178 DEG C～182 DEG C, Stress control is between 0.13Mpa～0.17Mpa, and fluohydric acid gas and phosphorus pentachloride react the mixing gas producing phosphorus pentafluoride and hydrogen chloride；
(2), the mixing gas of the phosphorus pentafluoride obtained and hydrogen chloride is passed in the reactor adding lithium fluoride and fluohydric acid gas liquid, between temperature controls 30 DEG C～35 DEG C, Stress control is between 0.6Mpa～0.7Mpa, reaction, obtain lithium hexafluorophosphate solution, wherein, the charged material weight of lithium fluoride, fluohydric acid gas liquid and phosphorus pentafluoride is than for 1:3～7:6～12；
(3), by gained lithium hexafluorophosphate solution through being filtered to remove insoluble impurities, filtrate is delivered in partial crystallization groove, it is cooled to-70 DEG C～-80 DEG C, lithium hexafluoro phosphate is made to precipitate out, filter, at temperature 50 C～70 DEG C, carry out one-level dry and obtain lithium hexafluoro phosphate crude product, after the lithium hexafluoro phosphate crude product obtained is pulverized according still further to Particle size requirements, at temperature 120 DEG C～130 DEG C, carry out secondary drying obtain lithium hexafluoro phosphate product.
Compared with prior art, it is an advantage of the current invention that:
The present invention passes through heater so that the fluohydric acid gas in fluohydric acid gas pipeline is in vaporized state all the time, and the fluohydric acid gas of gaseous state reacts with phosphorus pentachloride, decreases severe degree, and product quality is high.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present application or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, the accompanying drawing that the following describes is only some embodiments recorded in the application, for those of ordinary skill in the art, under the premise not paying creative work, it is also possible to obtain other accompanying drawing according to these accompanying drawings.
The structural representation that Fig. 1 show in the specific embodiment of the invention phosphorus pentafluoride reactor.
Detailed description of the invention
The present invention is described further by the following example: according to following embodiment, it is possible to be more fully understood that the present invention.But, as it will be easily appreciated by one skilled in the art that the concrete material ratio described by embodiment, process conditions and result thereof are merely to illustrate the present invention, and should without the present invention described in detail in restriction claims.
The preparation method of lithium hexafluoro phosphate, comprises the steps:
(1), hydrogen fluoride gas is passed in the reactor adding phosphorus pentachloride, temperature is controlled between 178 DEG C～182 DEG C, Stress control is between 0.13Mpa～0.17Mpa, and fluohydric acid gas and phosphorus pentachloride react the mixing gas producing phosphorus pentafluoride and hydrogen chloride；
(2), the mixing gas of the phosphorus pentafluoride obtained and hydrogen chloride is passed in the reactor adding lithium fluoride and fluohydric acid gas liquid, between temperature controls 30 DEG C～35 DEG C, Stress control is between 0.6Mpa～0.7Mpa, reaction, obtain lithium hexafluorophosphate solution, wherein, the charged material weight of lithium fluoride, fluohydric acid gas liquid and phosphorus pentafluoride is than for 1:3～7:6～12；
(3), by gained lithium hexafluorophosphate solution through being filtered to remove insoluble impurities, filtrate is delivered in partial crystallization groove, it is cooled to-70 DEG C～-80 DEG C, lithium hexafluoro phosphate is made to precipitate out, filter, at temperature 50 C～70 DEG C, carry out one-level dry and obtain lithium hexafluoro phosphate crude product, after the lithium hexafluoro phosphate crude product obtained is pulverized according still further to Particle size requirements, at temperature 120 DEG C～130 DEG C, carry out secondary drying obtain lithium hexafluoro phosphate product.
Hydrogen fluoride gas enters in reactor by pipeline, and owing to pipeline is long, fluohydric acid gas is easily lowered the temperature rapidly in the duct and become liquid, and it enters reactor and reacts violent with phosphorus pentachloride.
For this, this case embodiment arranges on pipeline heater so that pipe temperature is in more than 20 DEG C all the time.
Shown in Fig. 1, the phosphorus pentafluoride reactor in step (1) includes reactor 1 and the fluohydric acid gas pipeline 2 connected with reactor, and described fluohydric acid gas pipeline 2 is provided with heater 3.
Preferably, heater 3 is be set around electrical heating wire on described fluohydric acid gas pipeline or water circulation pipe.
Heater to fluohydric acid gas pipeline heating so that its temperature is more than hydrofluoric gasification temperature (20 DEG C).
Further, heater includes:
Temperature sensor, the in real time temperature in detection fluohydric acid gas pipeline, and this temperature information is sent to controller；
Controller 4, processes temperature information, and fluohydric acid gas pipeline is heated, and is positioned between setting district controlling temperature in pipeline.
Controller can include microprocessor (MCU), this MCU can include CPU (CentralProcessingUnit, CPU), read-only memory module (read-onlymemory, ROM), random memory module (randomaccessmemory, RAM), time block, digital-to-analogue conversion module (A/Dconverter) and plural number input/output port.Certainly, the integrated circuit that controller can also take other form, as: application-specific IC (ApplicationSpecificIntegratedCircuit, ASIC) or field programmable gate arrays (FieldProgrammableGateArray, FPGA) etc..
At this, in addition it is also necessary to explanation, in order to avoid having obscured the present invention because of unnecessary details, illustrate only in the accompanying drawings and according to the closely-related structure of the solution of the present invention and/or process step, and eliminate other details little with relation of the present invention.
Finally, it can further be stated that, term " includes ", " comprising " or its any other variant are intended to comprising of nonexcludability, so that include the process of a series of key element, method, article or equipment not only include those key elements, but also include other key elements being not expressly set out, or also include the key element intrinsic for this process, method, article or equipment.
Claims (7)
1. a phosphorus pentafluoride reactor, it is characterised in that include reactor and the fluohydric acid gas pipeline connected with reactor, described fluohydric acid gas pipeline is provided with heater.
2. phosphorus pentafluoride reactor according to claim 1, it is characterised in that: described heater is be set around electrical heating wire on described fluohydric acid gas pipeline or water circulation pipe.
3. phosphorus pentafluoride reactor according to claim 1, it is characterised in that: described heater to fluohydric acid gas pipeline heating so that its temperature is more than hydrofluoric gasification temperature.
4. phosphorus pentafluoride reactor according to claim 1, it is characterised in that: described heater includes:
Temperature sensor, the in real time temperature in detection fluohydric acid gas pipeline, and this temperature information is sent to controller；
Controller, processes temperature information, and fluohydric acid gas pipeline is heated, and is positioned between setting district controlling temperature in pipeline.
5. the preparation method of a phosphorus pentafluoride, it is characterised in that including:
(1), phosphorus pentachloride is put in reactor；
(2), passing in reactor by the fluohydric acid gas after gasification, reaction obtains phosphorus pentafluoride.
6. the preparation method of phosphorus pentafluoride according to claim 5, it is characterised in that: in described step (2), reaction temperature is 178～182 DEG C, and reaction pressure is 0.13～0.17MPa.
7. the preparation method of a lithium hexafluoro phosphate, it is characterised in that: comprise the steps:
(1), hydrogen fluoride gas is passed in the reactor adding phosphorus pentachloride, temperature is controlled between 178 DEG C～182 DEG C, Stress control is between 0.13Mpa～0.17Mpa, and fluohydric acid gas and phosphorus pentachloride react the mixing gas producing phosphorus pentafluoride and hydrogen chloride；
(2), the mixing gas of the phosphorus pentafluoride obtained and hydrogen chloride is passed in the reactor adding lithium fluoride and fluohydric acid gas liquid, between temperature controls 30 DEG C～35 DEG C, Stress control is between 0.6Mpa～0.7Mpa, reaction, obtain lithium hexafluorophosphate solution, wherein, the charged material weight of lithium fluoride, fluohydric acid gas liquid and phosphorus pentafluoride is than for 1:3～7:6～12；
(3), by gained lithium hexafluorophosphate solution through being filtered to remove insoluble impurities, filtrate is delivered in partial crystallization groove, it is cooled to-70 DEG C～-80 DEG C, lithium hexafluoro phosphate is made to precipitate out, filter, at temperature 50 C～70 DEG C, carry out one-level dry and obtain lithium hexafluoro phosphate crude product, after the lithium hexafluoro phosphate crude product obtained is pulverized according still further to Particle size requirements, at temperature 120 DEG C～130 DEG C, carry out secondary drying obtain lithium hexafluoro phosphate product.
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| CN201610235238.1A CN105731413A (en) | 2016-04-15 | 2016-04-15 | Phosphorus pentafluoride reaction still, phosphorus pentafluoride and preparation method for lithium hexafluorophosphate |
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| CN201610235238.1A CN105731413A (en) | 2016-04-15 | 2016-04-15 | Phosphorus pentafluoride reaction still, phosphorus pentafluoride and preparation method for lithium hexafluorophosphate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147436A (en) * | 2018-02-26 | 2018-06-12 | 江苏新泰材料科技有限公司 | Combined coefficient is improved in lithium hexafluoro phosphate production process reduces the synthetic method of unit consumption |
| CN115636429A (en) * | 2022-12-07 | 2023-01-24 | 山东立中新能源材料有限公司 | Preparation process of lithium hexafluorophosphate |
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| JPH0656413A (en) * | 1992-08-10 | 1994-03-01 | Central Glass Co Ltd | Production of hexafluorophosphate salt |
| CN102009972A (en) * | 2010-11-19 | 2011-04-13 | 森田化工(张家港)有限公司 | Preparation method of lithium hexafluorophosphate |
| CN102105394A (en) * | 2008-08-08 | 2011-06-22 | 斯泰拉化工公司 | Processes for production of phosphorus pentafluoride and hexafluorophosphates |
| CN102976297A (en) * | 2012-12-20 | 2013-03-20 | 天津隆尔新材料科技有限公司 | External circulation reactor and method for continuously preparing phosphorus pentafluoride |
| CN205500788U (en) * | 2016-04-15 | 2016-08-24 | 森田新能源材料（张家港）有限公司 | Phosphorus pentafluoride reation kettle |
-
2016
- 2016-04-15 CN CN201610235238.1A patent/CN105731413A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH0656413A (en) * | 1992-08-10 | 1994-03-01 | Central Glass Co Ltd | Production of hexafluorophosphate salt |
| CN102105394A (en) * | 2008-08-08 | 2011-06-22 | 斯泰拉化工公司 | Processes for production of phosphorus pentafluoride and hexafluorophosphates |
| CN102009972A (en) * | 2010-11-19 | 2011-04-13 | 森田化工(张家港)有限公司 | Preparation method of lithium hexafluorophosphate |
| CN102976297A (en) * | 2012-12-20 | 2013-03-20 | 天津隆尔新材料科技有限公司 | External circulation reactor and method for continuously preparing phosphorus pentafluoride |
| CN205500788U (en) * | 2016-04-15 | 2016-08-24 | 森田新能源材料（张家港）有限公司 | Phosphorus pentafluoride reation kettle |
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| 刘秀喜等: "《高纯气体的性质、制造和应用》", 30 June 1997 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147436A (en) * | 2018-02-26 | 2018-06-12 | 江苏新泰材料科技有限公司 | Combined coefficient is improved in lithium hexafluoro phosphate production process reduces the synthetic method of unit consumption |
| CN115636429A (en) * | 2022-12-07 | 2023-01-24 | 山东立中新能源材料有限公司 | Preparation process of lithium hexafluorophosphate |
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Application publication date: 20160706 |