CN109052349A - The continuous preparation method of phosphorus pentafluoride - Google Patents
The continuous preparation method of phosphorus pentafluoride Download PDFInfo
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- CN109052349A CN109052349A CN201811318499.5A CN201811318499A CN109052349A CN 109052349 A CN109052349 A CN 109052349A CN 201811318499 A CN201811318499 A CN 201811318499A CN 109052349 A CN109052349 A CN 109052349A
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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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Abstract
The present invention relates to the continuous preparation methods of phosphorus pentafluoride, belong to the preparation technical field of phosphorus pentafluoride.The technical problem to be solved by the present invention is to provide a kind of continuous preparation method of phosphorus pentafluoride, this method is passed through fluorine gas on the liquid level of liquid phosphor and carries out reaction production phosphorus pentafluoride, keep yellow phosphorus liquid level constant area in reaction process in inert gas shielding.The method of the present invention, it can be reacted by being continuously passed through fluorine gas and liquid phosphorus, to which phosphorus pentafluoride continuously be prepared, and the gas-solid reaction of traditional fluorine gas and phosphorus is become into gas liquid reaction, it reacts easily controllable, control gas flow and liquid levels area speed control can be passed through, achieve the purpose that control reaction heat, stablize entire reaction process, avoid explosion accident caused by vigorous reaction, reduces security risk.
Description
Technical field
The present invention relates to the continuous preparation methods of phosphorus pentafluoride, belong to the preparation technical field of phosphorus pentafluoride.
Background technique
Phosphorus pentafluoride is a kind of important inorganic fluoride, can be used for electronics industry, high molecular material and organic conjunction
At catalyst.In recent years, with the development of lithium battery, phosphorus pentafluoride is as production lithium cell electrolyte hexafluorophosphoric acid lithium material
Important source material, demand and quality requirements also increasingly improve, and therefore, large-scale continuous production phosphorus pentafluoride has extremely important
Meaning.
Currently, can be realized there are mainly two types of the techniques of industrialized production high-purity phosphorus pentafluoride, one is utilize pentachloro-
Change phosphorus and hydrogen fluoride reaction, generate phosphorus pentafluoride and hydrogen chloride, another kind is to generate five fluorinations using fluorine gas and simple substance phosphorus reaction
Phosphorus.Wherein, fluorine gas is reacted with elemental phosphorous since its reaction is very violent, releases big calorimetric, and reaction process is not easy to control, causes
Its technique controlling difficulty is larger, to mostly be intermittent production, can not accomplish serialization.
Application No. is 201210113224.4 patents of invention to disclose a kind of phosphorus pentafluoride continuous production device and side
Method, this method send the online continuously feeding phosphorus simple substance into fluorine phosphorus reaction device using spiral, while being passed through fluorine gas with specific flow velocity
It is reacted with phosphorus simple substance, the phosphorus pentafluoride gas of high-purity is obtained by filtration in the gas of generation after cooling pipe.This method
Due to being used as raw material using solid phosphorus, solid yellow phosphorus is the different particle of surface area, different moments be passed through reactor yellow phosphorus and
The contact area of fluorine gas cannot keep unanimously, and reaction rate is caused to have biggish fluctuation, is unfavorable for stablizing, accurately control instead
Rate is answered, since yellow phosphorus can discharge a large amount of heat with reacting for fluorine gas, when reaction rate fluctuation is larger, it is easy to react
Out of control and lead to explosion accident, security risk is larger.
Summary of the invention
For disadvantages described above, the technical problem to be solved by the present invention is to provide a kind of continuous preparation method of phosphorus pentafluoride,
The reaction process of this method is stable, security risk is smaller.
The continuous preparation method of phosphorus pentafluoride of the present invention leads on the liquid level of liquid phosphor in inert gas shielding
Enter fluorine gas and carry out reaction production phosphorus pentafluoride, keeps yellow phosphorus liquid level constant area in reaction process.
Preferably, yellow phosphorus liquid level area is 0.1~10m2, the speed that is passed through of fluorine gas is 0.5~10m/s.
Preferably, yellow phosphorus liquid level area is 0.1~2m2, the speed that is passed through of fluorine gas is 0.5~2m/s.
Preferably, the be passed through mouth and the spacing of yellow phosphorus liquid level of fluorine gas are 0.05m~1m.
Preferably, the be passed through mouth and the spacing of yellow phosphorus liquid level of fluorine gas are 50~120mm.
Preferably, reaction temperature is 80~250 DEG C.
It is furthermore preferred that reaction temperature is 100~200 DEG C.
Preferably, the inert gas is nitrogen, helium, neon, argon gas or Krypton.
Compared with prior art, the invention has the following beneficial effects:
The method of the present invention can be reacted by being continuously passed through fluorine gas and liquid phosphorus, to continuously be prepared into
Become gas liquid reaction to phosphorus pentafluoride, and by the gas-solid reaction of traditional fluorine gas and phosphorus, reacts easily controllable, can pass through
It controls gas flow and liquid levels area and speed control, achievees the purpose that control reaction heat, stablize entire reaction process,
Explosion accident caused by vigorous reaction is avoided, security risk is reduced.
Detailed description of the invention
Fig. 1 is schematic front view of the invention.
Fig. 2 is schematic top plan view of the invention.
Appended drawing reference: 1-horizontal reacting container；2-liquid level maintaining segment；3-feed pathways；4-inlet channels；5-rows
Gas channel；10-temperature detectors；11-pressure detectors.
Specific embodiment
The continuous preparation method of phosphorus pentafluoride of the present invention leads on the liquid level of liquid phosphor in inert gas shielding
Enter fluorine gas and carry out reaction production phosphorus pentafluoride, keeps yellow phosphorus liquid level constant area in reaction process.
The method of the present invention is reacted with fluorine gas after yellow phosphorus liquefaction, the gas-solid reaction of original fluorine gas and phosphorus is become
Gas liquid reaction reacts easily controllable, can reach control by the liquid level area speed control of control gas flow and liquid
The purpose of reaction heat processed stablizes entire reaction process, avoids explosion accident caused by vigorous reaction, reduces security risk.
And liquid phosphor can be passed through by the way that pipeline is lasting, fluorine gas can also be passed through by the way that pipeline is lasting, the phosphorus pentafluoride of production
Gas can be discharged by exhaust pipe, be achieved in the production of serialization.
In order to reduce reaction heat as far as possible, it is preferred that yellow phosphorus liquid level area is 0.1~10m2, fluorine gas is passed through speed
For 0.5~10m/s
Preferably, yellow phosphorus liquid level area is 0.1~2m2, the speed that is passed through of fluorine gas is 0.5~2m/s.
It after fluorine gas is contacted with liquid phosphorus liquid level, can quickly react, generate phosphorus pentafluoride.Preferably, fluorine gas is logical
The spacing of entrance and yellow phosphorus liquid level is 0.05m~1m.
Preferably, the be passed through mouth and the spacing of yellow phosphorus liquid level of fluorine gas are 50~120mm.
Since the reaction of fluorine gas and phosphorus is violent, reaction will release big calorimetric, and therefore, reaction temperature will be to the company of production
Continuous and temperature has an impact.Temperature is excessively high, and reaction speed is fast, will will cause production accident if heat release is fast, and temperature is too low, instead
Should will be insufficient, by-products content is high.It is preferred, therefore, that reaction temperature is 80~250 DEG C, more preferably 100~200 DEG C.
In the present invention, the inert gas is the gas not reacted with phosphorus or fluorine gas, it is preferred that the inert gas
For nitrogen, helium, neon, argon gas or Krypton.
The method of the present invention can be carried out using conventional equipment.
A specific embodiment of the invention is further described below with reference to embodiment, is not therefore limited the present invention
System is among the embodiment described range.
Embodiment 1
As depicted in figs. 1 and 2, it carries out preparing phosphorus pentafluoride using following equipment and technique.The production equipment of use, including
Horizontal reacting container 1, with the liquid level maintaining segment 2 of certain altitude in the inner cavity of the horizontal reacting container 1, the liquid level is kept
The area equation of the horizontal cross-section of 2 arbitrary height positions of section, the lower section of the liquid level maintaining segment 2 is provided with feed pathway 3, top
1 one end of horizontal reacting container be provided with inlet channel 4, the other end is provided with exhaust passage 5.Horizontal reacting container 1 is using resistance to
The reactor of high temperature and pressure, for feed pathway 3 for liquid phosphor to be continuously passed through to horizontal reacting container 1, inlet channel 4 is used for will
Fluorine gas is continuously passed through horizontal reacting container 1, and exhaust passage 5 is used to react the phosphorus pentafluoride discharge generated.
It is first passed through enough inert gas argon gas into horizontal reacting container, the air in horizontal reacting container is discharged, benefit
Solid yellow phosphorus is heated as liquid with heating equipment, liquid phosphor is then passed through horizontal reacting container, controls yellow phosphorus liquid
Face constant area is 0.5m2.Again fluorine gas is passed through horizontal reacting container above yellow phosphorus liquid level, is merely able to fluorine gas and yellow phosphorus
Liquid level contact, it is excessive with the contact area of yellow phosphorus and lead to react excessively violent to avoid fluorine gas.The speed that is passed through of fluorine gas is
1m/s, cooling liquid inlet are passed through coolant liquid, and control reaction temperature is 120 DEG C.The spacing guarantor for being passed through mouth and yellow phosphorus liquid level of fluorine gas
It holds in 50~80mm.With the progress of reaction, the yellow phosphorus in horizontal reacting container 1 is constantly consumed, and yellow phosphorus liquid level can reduce, and is used
Delivery pump is passed through the liquid phosphor of supplement from feed pathway 3, realizes the production of serialization.Temperature detector 10 is horizontal for detecting
Reaction temperature in reaction vessel 1, pressure detector 11 are used to detect the reaction pressure in horizontal reacting container 1, pass through monitoring
It is found that reaction temperature fluctuates in 100~140 DEG C, and reaction pressure fluctuates in 0.1~0.2MPa using the technique, it is anti-
Answer the fluctuation of temperature and reaction pressure smaller, reacting balance carries out.
Embodiment 2
Using the equipment recorded in embodiment 1 carry out phosphorus pentafluoride at production, the only parameter of changing section, wherein control
Yellow phosphorus liquid level constant area is 0.1m2, the speed that is passed through of fluorine gas is 0.5m/s, and control reaction temperature is 100 DEG C.Fluorine gas is passed through
The spacing of mouth and yellow phosphorus liquid level is maintained at 50~80mm.Temperature detector 10 detects the reaction temperature in horizontal reacting container 1, pressure
Force detector 11 detects the reaction pressure in horizontal reacting container 1, by monitoring it is found that using the technique, reaction temperature exists
It is fluctuated in 80~120 DEG C, reaction pressure fluctuates in 0.1~0.2MPa, and the fluctuation of reaction temperature and reaction pressure is smaller, instead
It should steadily carry out.
Embodiment 3
Using the equipment recorded in embodiment 1 carry out phosphorus pentafluoride at production, the only parameter of changing section, wherein control
Yellow phosphorus liquid level constant area is 2m2, the speed that is passed through of fluorine gas is 2m/s, and control reaction temperature is 200 DEG C.Fluorine gas be passed through mouth with
The spacing of yellow phosphorus liquid level is maintained at 80~120mm.Temperature detector 10 detects the reaction temperature in horizontal reacting container 1, pressure
Detector 11 detects the reaction pressure in horizontal reacting container 1, by monitoring it is found that reaction temperature is 180 using the technique
It is fluctuated in~220 DEG C, reaction pressure fluctuates in 0.1~0.2MPa, and the fluctuation of reaction temperature and reaction pressure is smaller, reaction
It is steady to carry out.
Claims (8)
1. the continuous preparation method of phosphorus pentafluoride, it is characterised in that: in inert gas shielding, on the liquid level of liquid phosphor
It is passed through fluorine gas and carries out reaction production phosphorus pentafluoride, keep yellow phosphorus liquid level constant area in reaction process.
2. the continuous preparation method of phosphorus pentafluoride according to claim 1, it is characterised in that: yellow phosphorus liquid level area is
0.1~10m2, the speed that is passed through of fluorine gas is 0.5~10m/s.
3. the continuous preparation method of phosphorus pentafluoride according to claim 2, it is characterised in that: yellow phosphorus liquid level area is
0.1~2m2, the speed that is passed through of fluorine gas is 0.5~2m/s.
4. the continuous preparation method of described in any item phosphorus pentafluorides according to claim 1~3, it is characterised in that: fluorine gas
The spacing for being passed through mouth and yellow phosphorus liquid level is 0.05m~1m.
5. the continuous preparation method of phosphorus pentafluoride according to claim 4, it is characterised in that: fluorine gas is passed through mouth and Huang
The spacing of phosphorus liquid level is 50~120mm.
6. the continuous preparation method of phosphorus pentafluoride according to claim 1, it is characterised in that: reaction temperature be 80~
250℃。
7. the continuous preparation method of phosphorus pentafluoride according to claim 6, it is characterised in that: reaction temperature be 100~
200℃。
8. the continuous preparation method of described in any item phosphorus pentafluorides according to claim 1~7, it is characterised in that: described lazy
Property gas be nitrogen, helium, neon, argon gas or Krypton.
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| CN201811318499.5A CN109052349A (en) | 2018-11-07 | 2018-11-07 | The continuous preparation method of phosphorus pentafluoride |
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| CN201811318499.5A CN109052349A (en) | 2018-11-07 | 2018-11-07 | The continuous preparation method of phosphorus pentafluoride |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115106022A (en) * | 2022-06-20 | 2022-09-27 | 江苏九九久科技有限公司 | High-safety phosphorus pentafluoride generator for controlling reaction process by utilizing thermal deformation |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007513853A (en) * | 2003-11-28 | 2007-05-31 | ゾルファイ フルーオル ゲゼルシャフト ミット ベシュレンクテル ハフツング | Method for increasing the content of phosphorus pentafluoride in a phosphorus pentafluoride-hydrogen chloride mixture |
| CN101417791A (en) * | 2008-11-17 | 2009-04-29 | 袁翔云 | Technique for preparing phosphorus pentafluoride |
| CN102421702A (en) * | 2009-03-13 | 2012-04-18 | 霍尼韦尔国际公司 | Methods and reactor designs for producing phosphorus pentafluoride |
-
2018
- 2018-11-07 CN CN201811318499.5A patent/CN109052349A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2007513853A (en) * | 2003-11-28 | 2007-05-31 | ゾルファイ フルーオル ゲゼルシャフト ミット ベシュレンクテル ハフツング | Method for increasing the content of phosphorus pentafluoride in a phosphorus pentafluoride-hydrogen chloride mixture |
| CN101417791A (en) * | 2008-11-17 | 2009-04-29 | 袁翔云 | Technique for preparing phosphorus pentafluoride |
| CN102421702A (en) * | 2009-03-13 | 2012-04-18 | 霍尼韦尔国际公司 | Methods and reactor designs for producing phosphorus pentafluoride |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115106022A (en) * | 2022-06-20 | 2022-09-27 | 江苏九九久科技有限公司 | High-safety phosphorus pentafluoride generator for controlling reaction process by utilizing thermal deformation |
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