Continuous producing device and method of phosphorus pentafluoride

Abstract

The invention provides a continuous producing device of phosphorus pentafluoride, comprising a phosphorus single-substance closing silo, a spiral conveyer, a fluorine-phosphorus reactor, a cooling pipeline and a multi-grade filter. The continuous producing device of phosphorus pentafluoride is characterized in that the upper end of the spiral conveyer is connected to the lower end of the phosphorus single-substance closing silo, the tail end of the spiral conveyer is connected to the upper part of the fluorine-phosphorus reactor; one end of the fluorine-phosphorus reactor is connected with the cooling pipeline, and the other end of the cooling pipeline is connected with the multi-grade filter. The invention further provides a method for continuously producing phosphorus pentafluoride by using the device; the high-purity phosphorus pentafluoride gas is obtained by pre-reaction, continuous reaction, cooling and multi-grade filtering. According to the continuous producing device, the continuous production of phosphorus pentafluoride is realized; the continuous producing device has the advantages of being high in production efficiency, simple, safe and reliable in operation and good in product quality; the product purity can reach 99.8% above; therefore, the continuous producing device can be directly applied to the production of the lithium hexafluorophosphate.

Description

technical field

[0001] The invention relates to a device and a process for producing inorganic fluorides, in particular to a device and a process for continuously producing phosphorus pentafluoride. Background technique

[0002] Phosphorus pentafluoride is an important inorganic fluoride, which can be used in the electronics industry, polymer materials and organic synthesis catalysts. In recent years, high-performance lithium batteries have increasingly become a development trend. As an important raw material for the production of lithium hexafluorophosphate materials for lithium battery electrolytes, the demand and quality requirements are getting higher and higher. Therefore, large-scale continuous production of high-quality phosphorus pentafluoride is very important. significance.

[0003] At present, there are two main processes for industrialized production of high-purity phosphorus pentafluoride:

[0004] 1. Using PCl 5 React with HF to produce PF 5

[0005] PCl ...

Examples

Embodiment 1

[0041] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0042] (1) Pre-reaction

[0043] First, add red phosphorus with a particle size of 5mm, a moisture content of less than 0.01%, and a purity of 99.5% into the 350L inverted conical pp material closed silo 1 of phosphorus element through the phosphorus element feed pipe 6, and then inject pressure through the inert gas interface 5 0.1MPa high-purity nitrogen protection, turn on the screw feeder 2, and slowly feed through the feeding insertion tube 8 to the pressure of -0.1MPa 1m 3Red phosphorus is added to the protection device 7 in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protection device is a cylindrical protection device with an overflow opening at the upper end, until the elemental phosphorus overflows the protection device in the fluorophosphorus reactor 3. After installation 7, close the screw feeder 2.

[0044] Open th...

Embodiment 2

[0048] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0049] (1) Pre-reaction

[0050] First, add ground red phosphorus with a particle size of 0.2mm, moisture content of less than 0.01%, and a purity of 99.5% into the 350L inverted conical pp material closed silo 1 of phosphorus element through the phosphorus element feed pipe 6, and then pass through the inert gas The interface 5 is connected with high-purity nitrogen protection with a pressure of 0.1MPa, the screw feeder 2 is turned on, and the feeding insertion tube 8 is slowly fed into the 1m with a pressure of -0.1MPa. 3 Red phosphorus is added to the protection device 7 in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protection device is a cylindrical protection device with an overflow opening on the upper end, until the phosphorus element overflows the protection device in the fluorophosphorus reactor. After 7, close the scr...

Embodiment 3

[0055] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0056] (1) Pre-reaction

[0057] First, add red phosphorus with a particle size of 0.5mm, a moisture content of less than 0.01%, and a purity of 99% into the 350L inverted conical pp material closed silo 1 through the phosphorus element feed pipe 6, and then feed it through the inert gas interface 5 Protected by high-purity argon gas with a pressure of 0.1MPa, turn on the screw feeder 2 and pass through the feeding insertion tube 8, slowly to the 1m with a pressure of -0.1MPa 3 Red phosphorus is added to the hemispherical protective device 7 with an upper opening in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protective device is a hemispherical protective device with an overflow opening at the upper end until the elemental phosphorus overflows with fluorophosphorus. After the protection device 7 in the reactor, the screw feeder...

technical field

[0001] The invention relates to a device and a process for producing inorganic fluorides, in particular to a device and a process for continuously producing phosphorus pentafluoride. Background technique

[0002] Phosphorus pentafluoride is an important inorganic fluoride, which can be used in the electronics industry, polymer materials and organic synthesis catalysts. In recent years, high-performance lithium batteries have increasingly become a development trend. As an important raw material for the production of lithium hexafluorophosphate materials for lithium battery electrolytes, the demand and quality requirements are getting higher and higher. Therefore, large-scale continuous production of high-quality phosphorus pentafluoride is very important. significance.

[0003] At present, there are two main processes for industrialized production of high-purity phosphorus pentafluoride:

[0004] 1. Using PCl 5 React with HF to produce PF 5

[0005] PCl ...

Examples

Embodiment 1

[0041] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0042] (1) Pre-reaction

[0043] First, add red phosphorus with a particle size of 5mm, a moisture content of less than 0.01%, and a purity of 99.5% into the 350L inverted conical pp material closed silo 1 of phosphorus element through the phosphorus element feed pipe 6, and then inject pressure through the inert gas interface 5 0.1MPa high-purity nitrogen protection, turn on the screw feeder 2, and slowly feed through the feeding insertion tube 8 to the pressure of -0.1MPa 1m 3Red phosphorus is added to the protection device 7 in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protection device is a cylindrical protection device with an overflow opening at the upper end, until the elemental phosphorus overflows the protection device in the fluorophosphorus reactor 3. After installation 7, close the screw feeder 2.

[0044] Open th...

Embodiment 2

[0048] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0049] (1) Pre-reaction

[0050] First, add ground red phosphorus with a particle size of 0.2mm, moisture content of less than 0.01%, and a purity of 99.5% into the 350L inverted conical pp material closed silo 1 of phosphorus element through the phosphorus element feed pipe 6, and then pass through the inert gas The interface 5 is connected with high-purity nitrogen protection with a pressure of 0.1MPa, the screw feeder 2 is turned on, and the feeding insertion tube 8 is slowly fed into the 1m with a pressure of -0.1MPa. 3 Red phosphorus is added to the protection device 7 in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protection device is a cylindrical protection device with an overflow opening on the upper end, until the phosphorus element overflows the protection device in the fluorophosphorus reactor. After 7, close the scr...

Embodiment 3

[0055] A continuous production device and process for phosphorus pentafluoride, comprising the following steps:

[0056] (1) Pre-reaction

[0057] First, add red phosphorus with a particle size of 0.5mm, a moisture content of less than 0.01%, and a purity of 99% into the 350L inverted conical pp material closed silo 1 through the phosphorus element feed pipe 6, and then feed it through the inert gas interface 5 Protected by high-purity argon gas with a pressure of 0.1MPa, turn on the screw feeder 2 and pass through the feeding insertion tube 8, slowly to the 1m with a pressure of -0.1MPa 3 Red phosphorus is added to the hemispherical protective device 7 with an upper opening in the volumetric horizontal carbon steel material fluorophosphorus reactor 3. The protective device is a hemispherical protective device with an overflow opening at the upper end until the elemental phosphorus overflows with fluorophosphorus. After the protection device 7 in the reactor, the screw feeder...

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