CN108147382A - A kind of synthetic method of phosphorus pentachloride - Google Patents
A kind of synthetic method of phosphorus pentachloride Download PDFInfo
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- CN108147382A CN108147382A CN201810191367.4A CN201810191367A CN108147382A CN 108147382 A CN108147382 A CN 108147382A CN 201810191367 A CN201810191367 A CN 201810191367A CN 108147382 A CN108147382 A CN 108147382A
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- reaction
- chlorine
- phosphorus pentachloride
- phosphorus
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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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The present invention provides a kind of synthetic methods of phosphorus pentachloride, using liquid phosphorus trichloride and chlorine as raw material, lead under chlorine reaction, stirring and logical chlorine pressurize that the reaction was continued under agitated and normal pressure and stirring and negative pressure under the reaction was continued three phases, obtain the phosphorus pentachloride finished product that uniform granularity, good fluidity, content are high, residual phosphorus trichloride content is low.Synthesis technology equipment is simple, and products obtained therefrom is high-quality, has higher industrial production value.
Description
Technical field
The present invention relates to a kind of synthetic methods of phosphorus pentachloride, belong to inorganic chemical synthesis technical field.
Background technology
Phosphorus pentachloride is one of widely used phosphorus chloride, and chlorinating agent is widely used as in organic synthesis, catalyst, is taken off
Aqua etc. has the characteristics that react fast, product yield high, such as medicine intermediate 7-ACA, paranitrobenzoyl chloride, oxalyl
The synthesis of chlorine etc..In domain of inorganic chemistry, phosphorus pentachloride is widely used in the production of lithium cell electrolyte lithium hexafluoro phosphate etc..
The synthetic method of phosphorus pentachloride is reacted using phosphorus trichloride and chlorine as raw material, generally using chlorine and liquid trichlorine
Change the gas-liquid reaction method of phosphorus reaction.But phosphorus pentachloride product is solid, with the raising of phosphorus trichloride conversion ratio, system stirring
It is increasingly difficult to or even is difficult to stir.In order to make phosphorus trichloride, the reaction was complete as far as possible, and general use is passed through excessive chlorine chlorination,
It is passed through the method that dry carbon dioxide gas discharges remaining chlorine again after reaction.It is however even if in this way, residual in product
The content for staying phosphorus trichloride is still higher, and generally 0.05% or even more than 0.1%, and chlorine is also arranged and is not thorough, and leads to product
Particle is uneven, hygroscopicity is strong, poor fluidity etc..
The technique of existing production phosphorus pentachloride deposits in the product that residual phosphorus trichloride content is high, granularity is uneven, flowing
The shortcomings of property is poor.
Invention content
The object of the present invention is to provide a kind of synthetic method of phosphorus pentachloride, the phosphorus pentachloride product of this method production has
The characteristics of content is high, residual phosphorus trichloride content is low, uniform granularity, good fluidity, and equipment is simple, it is easy to control the quality.
In order to achieve the object of the present invention, the present invention provides a kind of synthetic method of phosphorus pentachloride, is passed through and stirs including chlorine
Synthetic reaction is carried out in the phosphorus trichloride mixed, it is characterised in that the synthetic reaction includes following three stages：
A, the liquid phosphorus trichloride in reactor, and the chlorine being continuously passed through by reactor bottom are stirred to react 1.5- under normal pressure
8.0 hours, reaction temperature was 50-110 DEG C, and speed of agitator is 30-120 revs/min.
B, after normal pressure leads to chlorine, the reaction was continued 10-80 minutes under stirring and logical chlorine pressurize, and the pressure of logical chlorine pressurize is
0.1-8 kilograms, reaction temperature is 50-90 DEG C.
C, after leading to chlorine pressurize, the reaction was continued 10-100 minutes under stirring and negative pressure, and negative pressure is 50-740 millimetress of mercury,
Reaction temperature is 40-80 DEG C.
In features described above, the pressure of the logical chlorine pressurize refers to the pressure indicated on pressure gauge, inside reactor it is absolute
Pressure is that the pressure increases atmospheric pressure, and the negative pressure that the reaction was continued under the stirring and negative pressure refers to the pressure shown on vacuum meter,
The pressure of inside reactor is that about 760 millimetres of mercury of an atmospheric pressure subtracts the pressure shown on vacuum meter, and negative pressure numerical value is bigger, i.e.,
Reading is bigger on vacuum meter, then the pressure of inside reactor is smaller, and vacuum degree is higher.
Chlorine under traditional normal pressure is continuously passed through the technique in the phosphorus trichloride that stirred from reactor bottom by the present invention,
It is appropriate to continue continuation negative pressure stirring after stirred under pressure leads to chlorine chlorination appropriate time and the logical chlorine of pressurization after leading to chlorine with normal pressure
Time combines, both ensured phosphorus trichloride as far as possible with chlorine reaction, also ensure a small amount of unreacted phosphorus trichloride and
Chlorine is removed as far as possible.The technical solution, which realizes, directly obtains high-content, low phosphorus trichloride residual, uniform granularity, stream
The phosphorus pentachloride product for the comprehensive performances requirements such as dynamic property is good.
Synthetic method equipment proposed by the present invention is simple, and the content of gained phosphorus pentachloride product is high, up to more than 99.0%, produces
Remaining phosphorus trichloride content is low in product, be 0.02% hereinafter, and uniform granularity, good fluidity, have higher industrialization
Productive value.
Specific embodiment
Raw materials used following embodiment is technical grade product, without being further purified.Product content and phosphorus trichloride contain
The fixed method according to national standard defined is measured to carry out.
The synthesis of 1 phosphorus pentachloride of embodiment
Under the stirring of normal pressure and 60 revs/min of rotating speeds, chlorine is continuously led to the flow of 0.63 kg/minute by reactor bottom
Enter in the reactor equipped with 500 kg liquid phosphorus trichlorides, keep 50-80 DEG C of reaction temperature, react 7.5 hours, reactor
Tail gas is absorbed with sodium hydroxide solution.After normal pressure leads to chlorine, confined reaction system continues to be passed through chlorine to 0.4 public affairs under stirring
Jin pressure, and keep the pressure 80 minutes, temperature is 50-80 DEG C.After logical chlorine pressurize, 200-300 millimetress of mercury is kept to bear
Pressure continues to be stirred to react 18 minutes, and temperature is 50-70 DEG C.Cooling discharging is packaged to be phosphorus pentachloride finished product, content 99.2%,
Phosphorus trichloride content 0.02% is hereinafter, uniform granularity, good fluidity.
The synthesis of 2 phosphorus pentachloride of embodiment
Under the stirring of normal pressure and 70 revs/min of rotating speeds, chlorine is continuously led to the flow of 1.57 kg/minutes by reactor bottom
Enter in the reactor equipped with 500 kg liquid phosphorus trichlorides, keep 60-90 DEG C of reaction temperature, react 3.0 hours, reactor
Tail gas is absorbed with sodium hydroxide solution.After normal pressure leads to chlorine, confined reaction system continues to be passed through chlorine to 2.5 public affairs under stirring
Jin pressure, and keep the pressure 45 minutes, temperature is 50-80 DEG C.After logical chlorine pressurize, 80-150 millimetres of mercury negative pressure is kept
Under continue to be stirred to react 50 minutes, temperature be 40-60 DEG C.Cooling discharging is packaged to be phosphorus pentachloride finished product, content 99.1%, and three
Chlorination phosphorus content 0.02% is hereinafter, uniform granularity, good fluidity.
The synthesis of 3 phosphorus pentachloride of embodiment
It is under the stirring of normal pressure and 110 revs/min of rotating speeds, chlorine is continuous by reactor bottom with the flow of 2.35 kg/minutes
It is passed through in the reactor equipped with 500 kg liquid phosphorus trichlorides, the reaction temperature of 70-90 DEG C of holding is reacted 2.0 hours, reaction
Device tail gas is absorbed with sodium hydroxide solution.After normal pressure leads to chlorine, confined reaction system continues to be passed through chlorine to 4.5 under stirring
Kilogram pressure, and keep the pressure 35 minutes, temperature is 60-80 DEG C.After logical chlorine pressurize, 600-700 millimetress of mercury are kept
Continue to be stirred to react 70 minutes under negative pressure, temperature is 55-75 DEG C.Cooling discharging is packaged to be phosphorus pentachloride finished product, content
99.3%, phosphorus trichloride content 0.02% is hereinafter, uniform granularity, good fluidity.
The synthesis of 4 phosphorus pentachloride of embodiment
Under the stirring of normal pressure and 40 revs/min of rotating speeds, chlorine is continuously led to the flow of 0.86 kg/minute by reactor bottom
Enter in the reactor equipped with 500 kg liquid phosphorus trichlorides, keep 90-105 DEG C of reaction temperature, react 5.5 hours, reactor
Tail gas is absorbed with sodium hydroxide solution.After normal pressure leads to chlorine, confined reaction system continues to be passed through chlorine to 6.5 public affairs under stirring
Jin pressure, and keep the pressure 18 minutes, temperature is 70-90 DEG C.After logical chlorine pressurize, 350-450 millimetress of mercury is kept to bear
Pressure continues to be stirred to react 90 minutes, and temperature is 45-65 DEG C.Cooling discharging is packaged to be phosphorus pentachloride finished product, content 99.3%,
Phosphorus trichloride content 0.02% is hereinafter, uniform granularity, good fluidity.
The industry it is to be understood by the skilled artisans that the present invention is not limited to the above embodiments, above-described embodiment and explanation
It is described in book simply to illustrate that the principle of the present invention.Without departing from the spirit and scope of the present invention, the present invention is gone back
Various changes and modifications are had, these are both fallen in the scope of protection of present invention.
Claims (7)
1. a kind of synthetic method of phosphorus pentachloride, is passed through in the phosphorus trichloride that stirred including chlorine and carries out synthetic reaction, special
Sign is that the synthetic reaction includes following three stages：
A, the liquid phosphorus trichloride in reactor, and the chlorine being continuously passed through by reactor bottom are stirred to react 1.5- under normal pressure
8.0 hour；
B, after normal pressure leads to chlorine, the reaction was continued 10-80 minutes under stirring and logical chlorine pressurize；
C, after leading to chlorine pressurize, the reaction was continued 10-100 minutes under stirring and negative pressure.
2. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Phosphorus pentachloride synthetic reaction described in stage A
Temperature be 50-110 DEG C.
3. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Phosphorus pentachloride synthetic reaction described in stage A
Speed of agitator be 30-120 revs/min.
4. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Described in stage B under stirring and logical chlorine pressurize
The pressure that the reaction was continued is 0.1-8 kilograms.
5. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Described in stage B under stirring and logical chlorine pressurize
The reaction temperature that the reaction was continued is 50-90 DEG C.
6. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Continue under stirring and negative pressure described in stage C
The negative pressure of reaction is 50-740 millimetress of mercury.
7. phosphorus pentachloride synthetic method as described in claim 1, it is characterized in that：Continue under stirring and negative pressure described in stage C
The reaction temperature of reaction is 40-80 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201810191367.4A CN108147382A (en) | 2018-03-08 | 2018-03-08 | A kind of synthetic method of phosphorus pentachloride |
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| CN201810191367.4A CN108147382A (en) | 2018-03-08 | 2018-03-08 | A kind of synthetic method of phosphorus pentachloride |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
| CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420349A (en) * | 2012-05-21 | 2013-12-04 | 何猛 | Production method of phosphorus pentachloride |
| CN107117591A (en) * | 2017-06-27 | 2017-09-01 | 徐州江海源精细化工有限公司 | A kind of synthetic method of phosphorus pentachloride |
-
2018
- 2018-03-08 CN CN201810191367.4A patent/CN108147382A/en not_active Withdrawn
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103420349A (en) * | 2012-05-21 | 2013-12-04 | 何猛 | Production method of phosphorus pentachloride |
| CN107117591A (en) * | 2017-06-27 | 2017-09-01 | 徐州江海源精细化工有限公司 | A kind of synthetic method of phosphorus pentachloride |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113353958A (en) * | 2021-07-29 | 2021-09-07 | 上海绿麟达新材料科技有限公司 | Clean production process of hexafluorophosphate |
| CN114956021A (en) * | 2021-11-22 | 2022-08-30 | 上海绿麟达新材料科技有限公司 | Preparation method of phosphorus pentachloride |
| CN114956021B (en) * | 2021-11-22 | 2024-06-04 | 江西吉翔医药化工有限公司 | Preparation method of phosphorus pentachloride |
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