CN114604833A - Preparation method and application of phosphorus pentafluoride - Google Patents
Preparation method and application of phosphorus pentafluoride Download PDFInfo
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Abstract
The invention relates to the technical field of fluorine chemical industry, in particular to a preparation method and application of phosphorus pentafluoride. The invention provides a preparation method of phosphorus pentafluoride, which comprises the following steps: 1) adding phosphorus pentoxide into anhydrous hydrogen fluoride, adding sulfur trioxide into a reaction system after the phosphorus pentoxide is added, and heating for reaction to obtain a mixed gas containing phosphorus pentafluoride; 2) and condensing the mixed gas containing the phosphorus pentafluoride to obtain the phosphorus pentafluoride. According to the invention, the high-purity phosphorus pentafluoride can be obtained by controlling the adding sequence of phosphorus pentaoxide and anhydrous hydrogen fluoride and introducing sulfur trioxide as raw materials, heating for reaction and condensation, so that the content of water and hydrogen fluoride in the phosphorus pentafluoride is remarkably reduced, and meanwhile, the conversion rate of the phosphorus pentaoxide can reach 100%.
Description
Technical Field
The invention relates to the technical field of fluorine chemical industry, in particular to a preparation method and application of phosphorus pentafluoride.
Background
Phosphorus pentafluoride is a colorless gas, the melting point and the boiling point of the phosphorus pentafluoride are-94 ℃ and-84 ℃ respectively at normal pressure, the phosphorus pentafluoride is industrially used as a fluorinating agent to be applied to the fields of electronic industry and polymer material manufacturing, and can be used as a catalytic fluorinating agent in the field of organic synthesis.
In recent years, with the increasing popularization and promotion of high-performance mobile electronic products, the demand for high-performance secondary batteries is higher, lithium ion secondary batteries using lithium hexafluorophosphate as an electrolyte are widely used due to many advantages, and phosphorus pentafluoride gas is newly applied as a raw material for synthesizing lithium hexafluorophosphate. However, the production of lithium hexafluorophosphate places higher demands on the purity of phosphorus pentafluoride, and the synthesis of high purity phosphorus pentafluoride is undoubtedly of great significance for the synthesis of lithium hexafluorophosphate.
At present, the phosphorus pentafluoride preparation method is classified according to raw materials, and the phosphorus pentafluoride preparation method mainly comprises three types, namely a phosphorus pentachloride method, wherein PCl is used in the method5，PCl5In which a certain amount of water, phosphoric acid, etc. are often contained, plus synthetic PF5Corrosive HCl is generated in the process, the corrosion of equipment is greatly enhanced, higher requirements on the reliability of the equipment are provided, and the environmental protection pressure is high during industrial production. The second method adopts fluorine gas method, because the method uses simple substance fluorine, the danger of production link is large, the energy consumption of production process is high, and the cost is high. And the third method is a fuming sulfuric acid method, and the phosphorus pentafluoride obtained by the method has low purity and high hydrogen fluoride content, so that the application range of the phosphorus pentafluoride is limited.
Disclosure of Invention
Therefore, the technical problem to be solved by the invention is to overcome the defects of low purity and high hydrogen fluoride content of phosphorus pentafluoride obtained by adopting a fuming sulfuric acid method to prepare phosphorus pentafluoride in the existing phosphorus pentafluoride preparation method, and further provide a preparation method and application of phosphorus pentafluoride.
The invention provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
1) adding phosphorus pentoxide into anhydrous hydrogen fluoride, adding sulfur trioxide into a reaction system after the phosphorus pentoxide is added, and heating for reaction to obtain a mixed gas containing phosphorus pentafluoride;
2) and condensing the mixed gas containing the phosphorus pentafluoride to obtain the phosphorus pentafluoride.
Preferably, the step 1) is carried out under the protection of nitrogen or inert gas in the process of adding the phosphorus pentoxide into the anhydrous hydrogen fluoride, the temperature of the reaction system is controlled to be-10-20 ℃, and the pressure of the reaction system is 0.01-0.2 MPaG.
Preferably, the step 1) is carried out under the protection of nitrogen or inert gas in the process of adding sulfur trioxide into the reaction system, the temperature of the reaction system is controlled to be-10-20 ℃, and the pressure of the reaction system is 0.01-0.2 MPaG.
Preferably, the molar ratio of the phosphorus pentoxide to the anhydrous hydrogen fluoride is 1: (12-20); the molar ratio of the phosphorus pentoxide to the sulfur trioxide is 1: (4.8-5.2).
Preferably, the molar ratio of the phosphorus pentoxide to the sulfur trioxide is 1: (4.9-5.1).
Preferably, the heating reaction temperature is 100-140 ℃, and the heating reaction time is 0.5-1 h.
Preferably, the heating rate is controlled to be 10-18 ℃/h in the process of heating the reaction temperature to 100-140 ℃.
Preferably, the temperature rise rate is controlled to be 14-16 ℃/h.
Preferably, the condensation step is carried out in a reflux condensation tower, the temperature of the outlet of the reflux condensation tower is controlled to be-82 ℃ to-45 ℃, and the temperature of the cooling liquid in the reflux condensation tower is controlled to be-87 ℃ to-50 ℃.
Preferably, the outlet temperature of the reflux condensing tower is-80 ℃ to-50 ℃.
Preferably, the system pressure in the whole process of temperature rise, heating reaction and condensation is stably controlled to be 0.025-0.20 MPaG.
Preferably, in the step 1), the temperature of the reaction system is controlled to be-8-18 ℃ in the process of adding the phosphorus pentoxide into the anhydrous hydrogen fluoride; the molar ratio of the phosphorus pentoxide to the anhydrous hydrogen fluoride is 1: (13.5-18.5).
Preferably, the temperature of the reaction system is controlled to be-6 ℃ to 15 ℃ during the addition of sulfur trioxide to the reaction system in step 1).
The phosphorus pentafluoride prepared by the invention can be absorbed by high-purity water.
The invention also provides application of the phosphorus pentafluoride prepared by the preparation method in preparation of lithium hexafluorophosphate.
The technical scheme of the invention has the following advantages:
the invention provides a preparation method of phosphorus pentafluoride, which comprises the steps of adding phosphorus pentoxide into anhydrous hydrogen fluoride, adding sulfur trioxide into a reaction system after the phosphorus pentoxide is added, and heating for reaction to obtain a mixed gas containing phosphorus pentafluoride; and condensing the mixed gas containing the phosphorus pentafluoride to obtain the phosphorus pentafluoride. According to the invention, by controlling the adding sequence of phosphorus pentoxide and anhydrous hydrogen fluoride and introducing sulfur trioxide as raw materials, high-purity phosphorus pentafluoride can be obtained through heating reaction and condensation, the contents of water and hydrogen fluoride in the phosphorus pentafluoride are remarkably reduced, and meanwhile, the conversion rate of the phosphorus pentoxide can reach 100%.
The preparation method of phosphorus pentafluoride provided by the invention has the advantages of simple process, easily available raw materials, high product purity, high raw material utilization rate, convenience for industrial production and the like. Compared with the prior art, the method has obvious advantages and high economic and social benefits.
2) The preparation method of phosphorus pentafluoride provided by the invention further comprises the step 1) of adding phosphorus pentoxide into anhydrous hydrogen fluoride under the protection of nitrogen or inert gas, controlling the temperature of a reaction system to be-10-20 ℃, the pressure of the reaction system to be 0.01-0.2 MPaG, adding sulfur trioxide into the reaction system under the protection of nitrogen or inert gas, controlling the temperature of the reaction system to be-10-20 ℃, and the pressure of the reaction system to be 0.01-0.2 MPaG.
3) The invention provides a preparation method of phosphorus pentafluoride, and further provides a method for preparing phosphorus pentafluoride by using phosphorus pentoxide and anhydrous hydrogen fluoride in a molar ratio of 1: (12-20); the molar ratio of the phosphorus pentoxide to the sulfur trioxide is 1: (4.8-5.2). The invention can further ensure that the obtained high-purity phosphorus pentafluoride has lower water and hydrogen fluoride content by controlling the raw material proportion.
Detailed Description
The following examples are provided to further understand the present invention, not to limit the scope of the present invention, but to provide the best mode, not to limit the content and the protection scope of the present invention, and any product similar or similar to the present invention, which is obtained by combining the present invention with other prior art features, falls within the protection scope of the present invention.
The examples do not show the specific experimental steps or conditions, and can be performed according to the conventional experimental steps described in the literature in the field. The reagents or instruments used are not indicated by manufacturers, and are all conventional reagent products which can be obtained commercially.
The properties and components of anhydrous hydrogen fluoride, phosphorus pentoxide and sulfur trioxide used in the examples and comparative examples of the present invention were as follows:
anhydrous hydrogen fluoride (colorless transparent liquid): comprising HF: 99.96 wt%, H2O：0.0031wt％，H2SiF6：0.0096wt％，SO2: 0.0062 wt% of non-volatile acid (as H)2SO4Counting): 0.0042 wt%;
phosphorus pentoxide (white powder): including P2O5：99.67wt％，NO3 -：0.01wt％，PO4 3-：0.20wt％，Fe：0.001wt％；
Sulfur trioxide (colorless transparent liquid): including SO3：99.78wt％，SO2: 0.15 wt%, Fe: 0.005 wt%, ash: 0.035 wt%.
Example 1
The embodiment provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
1) after the device is qualified in air tightness inspection, replacing the system by nitrogen and maintaining the micro-positive pressure of the system;
2) adding 18.75mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle, simultaneously opening an inlet and outlet valve of kettle jacket chilled water (the temperature of the chilled water is minus 25 ℃), controlling the temperature of the kettle by adjusting the opening degree of the outlet valve, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the change of the temperature of the kettle in the adding process, controlling the temperature of a reaction system to be 20 ℃ and the pressure of the reaction system to be 0.05MPaG until the phosphorus pentoxide is completely added, then slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be 10 ℃ and the pressure of the reaction system to be 0.04MPaG in the adding process until the sulfur trioxide is completely added, then closing the inlet and outlet valve of the kettle jacket chilled water, evacuating residual water in the reaction kettle, communicating a steam inlet and outlet pipeline, checking to confirm that a steam drain pipeline is smooth, checking to confirm that the low-temperature (the low-temperature is minus 85 ℃) of a condensation reflux tower is normal, introducing water vapor (the vapor pressure is 0.6MPaG) into a jacket of a reaction kettle to increase the temperature of the kettle, controlling the flow of the vapor by adjusting an inlet valve to ensure that the temperature increase speed of the kettle is not too high, keeping the temperature increase speed at 14 ℃/h until the temperature of the kettle is increased to 100 ℃, reacting for 1h at 100 ℃, simultaneously enhancing and observing the temperature change condition of an outlet of a reflux condensing tower, controlling the temperature of the outlet of the reflux condensing tower to be-60 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, and condensing the mixed gas through the reflux condensing tower to obtain the phosphorus pentafluoride.
Example 2
The embodiment provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
1) after the device is qualified in air tightness inspection, the system is replaced by nitrogen, and the micro-positive pressure of the system is kept;
2) adding 21mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle, simultaneously opening a chilled water inlet and outlet valve of a kettle jacket (the temperature of the chilled water is-25 ℃), controlling the temperature of the kettle by adjusting the opening degree of the outlet valve, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the temperature change of the kettle in the adding process, controlling the temperature of a reaction system to be 15 ℃ and the pressure of the reaction system to be 0.04MPaG until the phosphorus pentoxide is completely added, then slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be 15 ℃ and the pressure of the reaction system to be 0.04MPaG in the adding process until the sulfur trioxide is completely added, then closing the chilled water inlet and outlet valve of the kettle jacket, emptying residual water in the reaction kettle, communicating a steam inlet and outlet pipeline side by side, checking and confirming that a steam drain pipeline is smooth, checking and confirming that the inlet and outlet of a condensing reflux tower are normal at low temperature (the low temperature is-85 ℃), introducing water vapor (the vapor pressure is 0.6MPaG) into a jacket of a reaction kettle to increase the temperature of the kettle, controlling the flow of the vapor by adjusting an inlet valve to ensure that the temperature increase speed of the kettle is not too high, keeping the temperature increase speed at 16 ℃/h until the temperature of the kettle is increased to 120 ℃, reacting for 1h at 120 ℃, simultaneously enhancing and observing the temperature change condition of an outlet of a reflux condensing tower, controlling the temperature of the outlet of the reflux condensing tower to be-75 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, and condensing the mixed gas through the reflux condensing tower to obtain the phosphorus pentafluoride.
Example 3
The embodiment provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
1) after the device is qualified in air tightness inspection, the system is replaced by nitrogen, and the micro-positive pressure of the system is kept;
2) adding 22.5mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle, simultaneously opening an inlet and outlet valve of kettle jacket chilled water (the temperature of the chilled water is minus 25 ℃), controlling the temperature of the kettle by adjusting the opening degree of the outlet valve, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the change of the temperature of the kettle in the adding process, controlling the temperature of a reaction system to be 15 ℃ and the pressure of the reaction system to be 0.04MPaG until the phosphorus pentoxide is completely added, then slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be 20 ℃ and the pressure of the reaction system to be 0.05MPaG in the adding process until the sulfur trioxide is completely added, then closing the inlet and outlet valve of the kettle jacket chilled water, evacuating residual water in the reaction kettle, communicating the residual water inlet and outlet pipeline with steam, checking to confirm that the steam drain pipeline is smooth, checking to confirm that the low-temperature (the low-temperature is minus 85 ℃) of the condensing reflux tower is normal, introducing water vapor (the vapor pressure is 0.6MPaG) into a jacket of a reaction kettle to increase the temperature of the kettle, controlling the flow of the vapor by adjusting an inlet valve to ensure that the temperature increase speed of the kettle is not too high, keeping the temperature increase speed at 18 ℃/h until the temperature of the kettle is increased to 140 ℃, reacting for 1h at 140 ℃, simultaneously enhancing and observing the temperature change condition of an outlet of a reflux condensing tower, controlling the temperature of the outlet of the reflux condensing tower to be-84 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, and condensing the mixed gas through the reflux condensing tower to obtain the phosphorus pentafluoride.
Example 4
The embodiment provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
adding 25.5mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle under the protection of nitrogen, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the temperature change of the reaction kettle in the adding process, controlling the temperature of a reaction system to be-8 ℃ and the pressure of the reaction system to be 0.04MPaG until the phosphorus pentoxide is completely added, then slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be-6 ℃ and the pressure of the reaction system to be 0.05MPaG in the adding process until the sulfur trioxide is completely added, then heating the reaction system, keeping the temperature rising speed at 16 ℃/h until the reaction system rises to 100 ℃, reacting for 1h at 100 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, condensing the mixed gas through a reflux condensing tower (the temperature of the cooling liquid in the reflux condensing tower is-85 ℃), and controlling the temperature of an outlet of the reflux condensing tower to be-80 ℃ to obtain the phosphorus pentafluoride.
Example 5
The embodiment provides a preparation method of phosphorus pentafluoride, which comprises the following steps:
adding 30mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle under the protection of nitrogen, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the temperature change of the reaction kettle in the adding process, controlling the temperature of the reaction system to be 18 ℃ and the pressure of the reaction system to be 0.04MPaG until the phosphorus pentoxide is completely added, then slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be 20 ℃ and the pressure of the reaction system to be 0.05MPaG in the adding process until the sulfur trioxide is completely added, then heating the reaction system, keeping the temperature rising speed at 14 ℃/h until the reaction system rises to 140 ℃, reacting for 1h at 140 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, condensing the mixed gas through a reflux condensing tower (the temperature of a cooling liquid in the reflux condensing tower is-55 ℃), and controlling the temperature of an outlet of the reflux condensing tower to be-50 ℃ to obtain the phosphorus pentafluoride.
Comparative example 1
The present comparative example provides a method for producing phosphorus pentafluoride, comprising the steps of:
adding 1.5mol of phosphorus pentoxide into a reaction kettle under the protection of nitrogen, adding 25.5mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into the reaction kettle, observing the temperature change of the reaction kettle in the adding process, controlling the temperature of a reaction system to be-8 ℃ and the pressure of the reaction system to be 0.04MPaG until the anhydrous hydrogen fluoride is completely added, slowly adding 7.5mol of sulfur trioxide into the reaction kettle, controlling the temperature of the reaction system to be-6 ℃ and the pressure of the reaction system to be 0.05MPaG in the adding process until the sulfur trioxide is completely added, heating the reaction system, keeping the temperature rising speed at 16 ℃/h until the reaction system rises to 100 ℃, reacting for 1h at 100 ℃, generating mixed gas containing phosphorus pentafluoride in the reaction process, condensing the mixed gas through a reflux condensing tower (the temperature of cooling liquid in the reflux condensing tower is-85 ℃), and controlling the temperature of an outlet of the reflux condensing tower to be-80 ℃ to obtain the phosphorus pentafluoride.
Comparative example 2
The present comparative example provides a method for producing phosphorus pentafluoride, comprising the steps of:
adding 25.5mol of anhydrous hydrogen fluoride (calculated by hydrogen fluoride) into a reaction kettle under the protection of nitrogen, then adding 1.5mol of phosphorus pentoxide into the reaction kettle, observing the temperature change of the reaction kettle in the adding process, controlling the temperature of a reaction system to be-8 ℃ and the pressure of the reaction system to be 0.04MPaG until the phosphorus pentoxide is completely added, then slowly adding 1000g of fuming sulfuric acid (the concentration of the fuming sulfuric acid is 60 wt%, and the sulfur trioxide in the fuming sulfuric acid is 7.5mol) into the reaction kettle, controlling the temperature of the reaction system to be-6 ℃ and the pressure of the reaction system to be 0.05MPaG in the adding process until the sulfur trioxide is completely added, then heating the reaction system, keeping the temperature rising speed at 16 ℃/h until the reaction system rises to 100 ℃, reacting for 1h at 100 ℃, and generating mixed gas containing the phosphorus pentafluoride in the reaction process, and condensing the mixed gas through a reflux condensing tower (the temperature of the cooling liquid in the reflux condensing tower is-85 ℃), and controlling the temperature of an outlet of the reflux condensing tower to be-80 ℃ to obtain the phosphorus pentafluoride.
Test example
The phosphorus pentafluoride gas components obtained in examples 1 to 5 and comparative examples 1 and 2 and the conversion of phosphorus pentoxide were subjected to test analysis.
The test results are shown in Table 1
TABLE 1
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (10)
1. A preparation method of phosphorus pentafluoride is characterized by comprising the following steps:
1) adding phosphorus pentoxide into anhydrous hydrogen fluoride, adding sulfur trioxide into a reaction system after the phosphorus pentoxide is added, and heating for reaction to obtain a mixed gas containing phosphorus pentafluoride;
2) and condensing the mixed gas containing the phosphorus pentafluoride to obtain the phosphorus pentafluoride.
2. The method according to claim 1, wherein the step 1) is carried out under protection of nitrogen or inert gas during addition of phosphorus pentoxide to anhydrous hydrogen fluoride, and the temperature of the reaction system is controlled to be-10 ℃ to 20 ℃ and the pressure of the reaction system is controlled to be 0.01 MPaG to 0.2 MPaG.
3. The method according to claim 1 or 2, wherein the step 1) is carried out under protection of nitrogen or inert gas during addition of sulfur trioxide into the reaction system, and the temperature of the reaction system is controlled to be-10 ℃ to 20 ℃ and the pressure of the reaction system is controlled to be 0.01 MPaG to 0.2 MPaG.
4. The method for producing phosphorus pentafluoride according to any one of claims 1 to 3,
the molar ratio of the phosphorus pentoxide to the anhydrous hydrogen fluoride is 1: (12-20); the molar ratio of the phosphorus pentoxide to the sulfur trioxide is 1: (4.8-5.2), preferably, the molar ratio of the phosphorus pentoxide to the sulfur trioxide is 1: (4.9-5.1).
5. The method according to any one of claims 1 to 4, wherein the heating reaction temperature is from 100 ℃ to 140 ℃ and the heating reaction time is from about 0.5 to 1 hour.
6. The method for producing phosphorus pentafluoride according to claim 5, wherein the temperature increase rate is controlled to 10 to 18 ℃/h, preferably 14 to 16 ℃/h, during the temperature increase of the reaction temperature to 100 to 140 ℃.
7. The method according to any one of claims 1 to 6, wherein the condensation step is carried out in a reflux condenser, and the outlet temperature of the reflux condenser is controlled to be from-82 ℃ to-45 ℃, the temperature of the cooling liquid in the reflux condenser is controlled to be from-87 ℃ to-50 ℃, and the preferred outlet temperature of the reflux condenser is controlled to be from-80 ℃ to-50 ℃.
8. The method of producing phosphorus pentafluoride according to any one of claims 1 to 6, wherein the temperature of the reaction system in the step 1) is controlled to be-8 ℃ to 18 ℃ during the addition of phosphorus pentoxide to anhydrous hydrogen fluoride; the molar ratio of the phosphorus pentoxide to the anhydrous hydrogen fluoride is 1: (13.5-18.5).
9. The production process of phosphorus pentafluoride according to any one of claims 1 to 8, wherein the temperature of the reaction system in the step 1) is controlled to-6 ℃ to 15 ℃ during addition of sulfur trioxide to the reaction system.
10. Use of phosphorus pentafluoride produced by the production method according to any one of claims 1 to 9 for producing lithium hexafluorophosphate.
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