CN102502544A - Preparation method of phosphorus pentafluoride - Google Patents
Preparation method of phosphorus pentafluoride Download PDFInfo
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- CN102502544A CN102502544A CN2011103291734A CN201110329173A CN102502544A CN 102502544 A CN102502544 A CN 102502544A CN 2011103291734 A CN2011103291734 A CN 2011103291734A CN 201110329173 A CN201110329173 A CN 201110329173A CN 102502544 A CN102502544 A CN 102502544A
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Abstract
The invention discloses a preparation method of phosphorus pentafluoride, which includes: (i) drying: removing water in a reactor and a pipeline, (ii) material adding: adding two solid powder of phosphorus pentoxide and calcium fluoride in the reactor under protection of inert gases in dry environment, (iii) vacuuming: vacuuming the reactor to -0.09MPa to -0.11MPa, (iv) synthetic reaction: controlling the reaction temperature within 200 DEG C to 300 DEG C, controlling pressure of the reactor within -0.1MPa to 0MPa, leading reaction time to be more than 3 hours so as to generate rough phosphorus pentafluoride gas, and (v) purification. The preparation method of phosphorus pentafluoride is simple in process and device and high in reliability, the process is easy to control, raw materials are non-toxic and easy to obtain, and product purity is as high as 99.9%. Another product Ca(PO3)2 is non-toxic and harmless and can be recycled.
Description
Technical field
The invention belongs to a kind of technology for preparing phosphorus pentafluoride, be specifically related to a kind of method of utilizing Vanadium Pentoxide in FLAKES and two kinds of solid reacting by heating of Calcium Fluoride (Fluorspan), preparing phosphorus pentafluoride.
Background technology
Phosphorus pentafluoride (PF
5) be a kind of gas of colorless and odorless under normal conditions, in damp atmosphere, acutely to be fuming, fusing point is-93.78 ° of C under the normal pressure, boiling point-84 ° C.As a kind of fluorizating agent, phosphorus pentafluoride can carry out ion-transfer, is widely used in fields such as electronic industry, battery manufacturing, macromolecular material and catalyzer.On semi-conductor was made, phosphorus pentafluoride became plasma gas and mixes and can significantly improve semiconducting behavior under microwave action.
At polymeric material field, phosphorus pentafluoride can synthesize as reactant fluoridizes organic disulfide for phosphoric acid salt, has the macromolecular material of fine antiseptic property in order to preparation.
Lithium cell is widely used at present, can be used as the power supply of electromobile, laptop computer, mobile telephone.Its electrolytical performance has very big influence to battery performance; With the phosphorus pentafluoride be raw material can prepare excellent performance lithium hexafluoro phosphate as electrolyte for Lithium Battery; Thereby can significantly improve the performance of lithium cell, work-ing life and charging times can greatly increase.
The oxide compound of metals such as the Al that handled with phosphorus pentafluoride, Ni, Be, Th, Ti is as catalyzer, and to the conversion of hydrocarbon compound, for example tributyl toluene is converted into toluene and has good catalytic performance.
Phosphorus pentafluoride also can directly be used as the catalyzer of many copolyreaction, like the copolyreaction of grape acid anhydride with the dehydration seminose.In addition, be that raw material can synthesize phosphorus pentafluoride amine copolymer thing as herbicide with phosphorus pentafluoride.
In view of this, phosphorus pentafluoride has purposes more widely.Particularly the high purity anhydrous phosphorus pentafluoride can directly be used for electronic industry.Therefore need find a kind of economical and efficient, the simple preparation method of technology.
At present, the preparation method of main phosphorus pentafluoride is broadly divided into direct method, indirect method.
It is raw material that direct method generally adopts hydrogen fluoride and fluorine gas etc., prepares phosphorus pentafluoride through single step reaction.For example: utilize fluorine gas and elemental phosphorous reaction to synthesize phosphorus pentafluoride, reaction equation is 2P+5F
22PF
5Vanadium Pentoxide in FLAKES and anhydrous hydrogen fluoride reaction prepare phosphorus pentafluoride, and reaction equation is PCl
5+ HF PF
5+ HCl; Halogen is with phosphorus trifluoride prepared in reaction phosphorus pentafluoride, and reaction equation is 5PF
3+ 3X
2→ 3PF
5+ 2PX
5(wherein X is a halogen); Fluorine gas and Vanadium Pentoxide in FLAKES prepared in reaction phosphorus pentafluoride, reaction equation is 2P
2O
5+ 10F
2→ 4PF
5+ 5O
2
Fluorine gas and hydrogen fluoride that above-mentioned reaction is adopted are to have severe corrosive and deleterious raw material, reactor drum had relatively high expectations, and also the reaction very exothermic, restive, be easy to generate by products such as phosphorus trifluoride, influence product purity.
Though the preparation method of Vanadium Pentoxide in FLAKES and anhydrous hydrogen fluoride reaction phosphorus pentafluoride has realized industrialization, this method of the many employings of the preparation of domestic commerce phosphorus pentafluoride.But because this strong reaction heat release needs strict control reaction process temperature, otherwise blasts easily.In addition, reaction yield is low.
Indirect production method is that to make an amount of reactant at first generate intermediate product (mainly be POF
3And HPF
6), middle product is handled the generation phosphorus pentafluoride.The working system reactions step is many indirectly, and difficulty is produced in serialization, and process step is complicated, and production cost is high.
(patent No.: US3592594) disclose a kind of indirect working system that utilizes intermediate product trifluoro oxygen phosphorus, reaction principle is CaF to USP
2Generate CaF (SO with the anhydrous sodium sulfuric acid reaction
3F), again with H
3PO
4Reaction generates trifluoro oxygen phosphorus.Continue to let trifluoro oxygen phosphorus and HF reaction generate PF
5Reaction equation is respectively: CaF
2+ H
2SO
3→ CaF (SO
3F)+H
2, 3CaF (SO
3F)+2H
3PO
4→ 3CaSO
4+ 2POF
3+ 3H
2O, POF
3+ 2HF → 2PF
5+ H
2O.
Aforesaid method once once had been the important method of traditional preparation process phosphorus pentafluoride, but because the byproduct of reaction environmental pollution is serious, nowadays this method is stopped using.
Summary of the invention
The objective of the invention is to use in the abandoning tradition working method strong toxicity such as hydrogen fluoride, fluorine gas and the raw-material way of severe corrosive, a kind of process method for preparing high purity phosphorus pentafluoride is provided.
Technical scheme of the present invention is: a kind of preparation method of phosphorus pentafluoride may further comprise the steps:
(i) drying
Be heated to 90～100 ° of C for the horizontal reactor of band whipping appts, kept 0.4～0.6 hour, remove the moisture in reactor drum and the pipeline;
(ⅱ) reinforced
In the exsiccant environment, under protection of inert gas, while hot pressed powder Vanadium Pentoxide in FLAKES and pressed powder Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts rapidly;
(ⅲ) find time
Closed reactor, the reactor drum of finding time to-0.09～-0.11MPa, close the valve of finding time, observe for some time, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation;
(ⅳ) building-up reactions
To the reactor drum heating, temperature of reaction is controlled at 200～300 ° of C, and reactor pressure is controlled at
-0.1～0 MPa, the reaction times is more than 3 hours, generates the phosphorus pentafluoride gas bullion;
Reaction equation is following:
6P
2O
5+5CaF
2→2PF
5+5Ca（PO
3）
2
(ⅴ) purify
After reacting by heating was complete, the phosphorus pentafluoride gas bullion of generation was removed O through the condensing surface cooling
2, N
2, CO
2Obtain highly purified phosphorus pentafluoride, the step of this condensation removal of impurities also can repeat 1 time or repeatedly.
The mass ratio that Vanadium Pentoxide in FLAKES and Calcium Fluoride (Fluorspan) add in building-up reactions is 2～2.5:1, and Vanadium Pentoxide in FLAKES is excessive.
Described synthesising reacting time 33 hours.
Described synthetic optimum reacting time 35 hours.
Described inert gas adopts nitrogen or argon gas.
The present invention has the following advantages: advantages of nontoxic raw materials, be easy to get, technological process and device structure are simple, and safety is high.The preparation process is easy to control.Reaction process is simple, and product is single, and product purity is high.Another kind of product C a (PO
3)
2Nontoxic, can recycle.
Embodiment
Below, in conjunction with embodiment the preparation method of phosphorus pentafluoride of the present invention is elaborated:
A kind of preparation method of phosphorus pentafluoride may further comprise the steps:
(i) drying
Be heated to 90～110 ° of C for the horizontal reactor of band whipping appts, kept 0.4～0.6 hour, remove the moisture in reactor drum and the pipeline.
(ⅱ) reinforced
In the exsiccant environment, under protection of inert gas, while hot pressed powder Vanadium Pentoxide in FLAKES and pressed powder Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts rapidly.
(ⅲ) find time
Closed reactor, the reactor drum of finding time to-0.09～-0.11MPa, close the valve of finding time, observe for some time, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation.
(ⅳ) building-up reactions
To the reactor drum heating, temperature of reaction is controlled at 200～300 ° of C, and reactor pressure is controlled at
-0.1～0 MPa, the reaction times is more than 3 hours, generates the phosphorus pentafluoride gas bullion.
Reaction equation is following:
6P
2O
5+5CaF
2→2PF
5+5Ca（PO
3）
2
Its by product is Ca (PO
3)
2, be solid residue, nontoxic.
Contain O in the bullion
2, N
2, CO
2Deng impurity.
(ⅴ) purify
After reacting by heating was complete, the phosphorus pentafluoride gas bullion of generation was removed O through the condensing surface cooling
2, N
2, CO
2, obtain highly purified phosphorus pentafluoride.The step of this condensation removal of impurities also can repeat 1 time or repeatedly.
Described solid-state Vanadium Pentoxide in FLAKES and Calcium Fluoride (Fluorspan) mass ratio are 2～2.5:1, and solid-state Vanadium Pentoxide in FLAKES is excessive.
Described horizontal reactor band whipping appts, material is a stainless steel.Described rare gas element adopts nitrogen or argon gas.Described condensing surface heat-eliminating medium adopts industrial spirit.Industrial spirit adopts liquid nitrogen to carry out freezing.
33 hours described reaction times, Best Times 35 hours.
Embodiment 1
Be heated to 90 ° of C for the horizontal reactor of band whipping appts, kept 0.4 hour, remove the moisture in reactor drum and the pipeline.
In the exsiccant environment, under protection of inert gas, while hot 1 kilogram of Vanadium Pentoxide in FLAKES and 0.5 kilogram of Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts closed reactor rapidly.Rare gas element adopts nitrogen.
Find time reactor drum to-0.09MPa, close the valve of finding time, observed 10 minutes, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation.
The formal reaction of beginning, to the reactor drum heating, temperature of reaction is controlled at 200 ° of C, and gaseous tension is controlled at-0.1～0 MPa, and the reaction times is 3 hours, generates the phosphorus pentafluoride gas bullion.
After reacting by heating was complete, product obtained highly purified phosphorus pentafluoride through condensing surface cooling removal of impurities.Heat-eliminating medium adopts alcohol, needs use liquid nitrogen to be solid with alcohol is freezing.The step of condensation removal of impurities repeats 2 times.The phosphorus pentafluoride product 180g that obtains, through analyzing, product purity is 99.9%.
Embodiment 2
Be heated to 100 ° of C for the horizontal reactor of band whipping appts, kept 0.5 hour, remove the moisture in reactor drum and the pipeline.
In the exsiccant environment, under protection of inert gas, while hot 2.25 kilograms of Vanadium Pentoxide in FLAKESs and 1 kilogram of Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts closed reactor rapidly.Rare gas element adopts nitrogen.
Find time reactor drum to-0.1MPa, close the valve of finding time, observed 10 minutes, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation.
The formal reaction of beginning, to the reactor drum heating, temperature of reaction is controlled at 250 ° of C, gaseous tension control-0.1～0 MPa, the reaction times is 5 hours, generates the phosphorus pentafluoride bullion.
After reacting by heating was complete, product obtained highly purified phosphorus pentafluoride through condensing surface cooling removal of impurities.Heat-eliminating medium adopts alcohol, needs use liquid nitrogen to be solid with alcohol is freezing.The step of condensation removal of impurities repeats 2 times.The phosphorus pentafluoride product 380g that obtains, through analyzing, product purity is 99.9%.
Embodiment 3
Be heated to about 100 ° of C for the solid gas-solids reactors of band whipping appts, kept 0.6 hour, remove the moisture in reactor drum and the pipeline.
In the exsiccant environment, under protection of inert gas, while hot 3.75 kilograms of Vanadium Pentoxide in FLAKESs and 1.5 kilograms of Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts closed reactor rapidly.Rare gas element adopts nitrogen.
Find time reactor drum to-0.11MPa, close the valve of finding time, observed 10 minutes, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation.
The formal reaction of beginning, to the reactor drum heating, temperature of reaction is controlled at 300 ° of C, gaseous tension control-0.1～0 MPa, the reaction times is 6 hours, generates the phosphorus pentafluoride bullion.
After reacting by heating was complete, product obtained highly purified phosphorus pentafluoride through condensing surface cooling removal of impurities.Heat-eliminating medium adopts alcohol, needs use liquid nitrogen to be solid with alcohol is freezing.The step of condensation removal of impurities repeats 3 times.The phosphorus pentafluoride product 570g that obtains, through analyzing, product purity is 99.9%.
Technological process of the present invention and equipment are simple, safety is high, process is easy to control, and product purity is high.Advantages of nontoxic raw materials, be easy to get.Another kind of product C a (PO
3)
2Nontoxic, can recycle.
Claims (5)
1. the preparation method of a phosphorus pentafluoride is characterized in that: may further comprise the steps:
(i) drying
Be heated to 90～110 ° of C for the horizontal reactor of band whipping appts, kept 0.4～0.6 hour, remove the moisture in reactor drum and the pipeline;
(ⅱ) reinforced
In the exsiccant environment, under protection of inert gas, while hot pressed powder Vanadium Pentoxide in FLAKES and pressed powder Calcium Fluoride (Fluorspan) are joined in the horizontal reactor of band whipping appts rapidly;
(ⅲ) find time
Closed reactor, the reactor drum of finding time to-0.09～-0.11MPa, close the valve of finding time, observe for some time, pressure does not go up and thinks that reactor drum does not leak, and can carry out following operation;
(ⅳ) building-up reactions
To the reactor drum heating, temperature of reaction is controlled at 200～300 ° of C, and reactor pressure is controlled at
-0.1～0 MPa, the reaction times is more than 3 hours, generates the phosphorus pentafluoride gas bullion;
Reaction equation is following:
6P
2O
5+5CaF
2→2PF
5+5Ca（PO
3）
2
(ⅴ) purify
After reacting by heating was complete, the phosphorus pentafluoride gas bullion of generation found time to remove O through the condensing surface cooling
2, N
2, CO
2Obtain highly purified phosphorus pentafluoride, the step of this condensation removal of impurities also can repeat 1 time or repeatedly.
2. the preparation method of phosphorus pentafluoride according to claim 1 is characterized in that: the mass ratio that Vanadium Pentoxide in FLAKES and Calcium Fluoride (Fluorspan) add in building-up reactions is 2～2.5:1, and Vanadium Pentoxide in FLAKES is excessive.
3. the preparation method of phosphorus pentafluoride according to claim 1 is characterized in that: described synthesising reacting time 33 hours.
4. the preparation method of phosphorus pentafluoride according to claim 1 is characterized in that: described best synthesising reacting time 35 hours.
5. the preparation method of phosphorus pentafluoride according to claim 1 is characterized in that: described rare gas element employing nitrogen or argon gas.
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| CN2011103291734A CN102502544A (en) | 2011-10-26 | 2011-10-26 | Preparation method of phosphorus pentafluoride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261369A (en) * | 2014-08-26 | 2015-01-07 | 九江天赐高新材料有限公司 | Preparation method of high purity phosphorus pentafluoride |
| CN108689886A (en) * | 2018-06-22 | 2018-10-23 | 湖北卓熙氟化股份有限公司 | A kind of preparation method of fluorination urea hydrogen |
| CN114057170A (en) * | 2021-12-20 | 2022-02-18 | 瓮福（集团）有限责任公司 | Method for synthesizing phosphorus pentafluoride and preparing lithium hexafluorophosphate by solid phase method |
Citations (1)
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|---|---|---|---|---|
| CN101391760A (en) * | 2008-10-28 | 2009-03-25 | 中南大学 | Method for preparing high purity phosphorus pentafluoride gas |
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2011
- 2011-10-26 CN CN2011103291734A patent/CN102502544A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101391760A (en) * | 2008-10-28 | 2009-03-25 | 中南大学 | Method for preparing high purity phosphorus pentafluoride gas |
Non-Patent Citations (1)
| Title |
|---|
| 刘建文等: "五氟化磷制备过程的GC-MS-SIM法评价与检测", 《中南大学学报（自然科学版）》, vol. 40, no. 4, 31 August 2009 (2009-08-31), pages 868 - 873 * |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104261369A (en) * | 2014-08-26 | 2015-01-07 | 九江天赐高新材料有限公司 | Preparation method of high purity phosphorus pentafluoride |
| CN108689886A (en) * | 2018-06-22 | 2018-10-23 | 湖北卓熙氟化股份有限公司 | A kind of preparation method of fluorination urea hydrogen |
| CN108689886B (en) * | 2018-06-22 | 2021-06-15 | 湖北卓熙氟化股份有限公司 | Preparation method of hydrogen fluoride urea |
| CN114057170A (en) * | 2021-12-20 | 2022-02-18 | 瓮福（集团）有限责任公司 | Method for synthesizing phosphorus pentafluoride and preparing lithium hexafluorophosphate by solid phase method |
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Application publication date: 20120620 |