CN108675274A - A kind of preparation method of high-purity phosphorus pentachloride - Google Patents
A kind of preparation method of high-purity phosphorus pentachloride Download PDFInfo
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- CN108675274A CN108675274A CN201811022336.2A CN201811022336A CN108675274A CN 108675274 A CN108675274 A CN 108675274A CN 201811022336 A CN201811022336 A CN 201811022336A CN 108675274 A CN108675274 A CN 108675274A
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- liquid
- chlorine
- carbon dioxide
- phosphorus pentachloride
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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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- Inorganic Chemistry (AREA)
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Abstract
The present invention discloses a kind of preparation method of high-purity phosphorus pentachloride, includes the following steps：1）Liquid chlorine and liquid carbon dioxide are sent by closed conduit in drying tower A and drying tower B containing physical dryness agent respectively, slough the moisture in liquid chlorine and liquid carbon dioxide respectively using physical dryness agent, dry liquid chlorine and liquid carbon dioxide is made, it is spare；2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and are stored in two surge tanks respectively, and chlorine and carbon dioxide is made, spare；3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorination reaction, wherein reaction temperature is controlled at 110 120 DEG C, and chlorine is passed through from reactor bottom, until becoming solid crystalline completely by liquid phase to material in reactor, stops leading to chlorine；Phosphorus pentachloride purity made from the preparation method of the high-purity phosphorus pentachloride is high, and impurity is few.
Description
Technical field
The present invention relates to a kind of preparation methods of high-purity phosphorus pentachloride.
Background technology
Phosphorus pentachloride is a kind of inorganic compound.It is one of most important phosphorus chloride, and others also have phosphorus trichloride
And phosphorus oxychloride.Pale yellow crystals, irritant smell easily distil.There can be different structures at different conditions.In organic conjunction
It is used as chlorinating agent, catalyst in.It is to produce the raw material of medicine, dyestuff, chemical fibre, and produce phosphonitrilic chloride, phosphoryl chloride phosphorus oxychloride
Raw material.
Current phosphorus pentachloride mainly uses liquid chlorine and phosphorus trichloride to make, and the purity for promoting phosphorus pentachloride is this field
Technical staff endeavours always the direction of research.
Invention content
The technical problem to be solved in the present invention is to provide a kind of preparation methods of high-purity phosphorus pentachloride.
To solve the above problems, the present invention adopts the following technical scheme that：
A kind of preparation method and preparation method thereof of high-purity phosphorus pentachloride, includes the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature control at 110-120 DEG C, chlorine is passed through from reactor bottom, until to material in reactor by
Liquid phase becomes solid crystalline completely, stops leading to chlorine, and crystal is made, spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 160-170
DEG C so that coarse crystal stands 20min completely after by heat sublimation；Then pumping process is carried out, using air pump by the gas in heating tank
Body is completely withdrawn into dustless tank, and gas filters before entering dustless tank by filter, and impurity trapped then carries out dustless tank
Cooling treatment so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
Preferably, filter is heated to 165 DEG C and keeps the temperature until arriving pumping process knot when the pumping process
Beam.
Preferably, the physical dryness agent is the mixing of sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini
Object.
Preferably, the vaporization process is hot the specific steps are liquid chlorine and liquid carbon dioxide are respectively fed to heat exchange
In device, heating water bath is used outside heat exchanger, it is 40-50 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide are abundant
Vaporization.
Preferably, when the chlorination reaction, the mixing speed of the agitating shaft of reaction kettle is 40-50r/min, until arriving object
Until material becomes solid crystalline completely by liquid phase.
Preferably, in the purge, the purging pressure of carbon dioxide is 3-6MPa.
Preferably, the sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini weight ratio be 2：1：1：1.
The beneficial effects of the invention are as follows：Remaining phosphorus trichloride is eliminated in the production process, and is utilized phosphoric
Phosphorus is easy the characteristics of by heat sublimation, and phosphorus pentachloride heating is become gaseous state, is then extracted into again in another dustless, clean tank
It is cooling so that phosphorus pentachloride becomes crystallization again again in this tank, and filtration treatment is additionally provided in whole process so that five
Phosphorus chloride is detached with impurity, effectively raises the purity of phosphorus pentachloride.
Specific implementation mode
Embodiment 1：
A kind of preparation method and preparation method thereof of high-purity phosphorus pentachloride, includes the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature is controlled at 110 DEG C, and chlorine is passed through from reactor bottom, until to material in reactor by liquid phase
Become solid crystalline completely, stop leading to chlorine, crystal is made, it is spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 160 DEG C, is made
It obtains coarse crystal and stands 20min completely after by heat sublimation；Then pumping process is carried out, it is using air pump that the gas in heating tank is complete
It is pumped into dustless tank, gas filters before entering dustless tank by filter, impurity trapped, then carries out cooling place to dustless tank
Reason so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
In the present embodiment, filter is heated to 165 DEG C and keeps the temperature until at pumping when the pumping process
Reason terminates.
In the present embodiment, the physical dryness agent is sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini
Mixture.
In the present embodiment, the vaporization process the specific steps are liquid chlorine and liquid carbon dioxide are respectively fed to hot friendship
In heat exchanger, heating water bath is used outside heat exchanger, it is 40 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide are abundant
Vaporization.
In the present embodiment, when the chlorination reaction, the mixing speed of the agitating shaft of reaction kettle is 40r/min, until arriving
Until material becomes solid crystalline completely by liquid phase.
In the present embodiment, in the purge, the purging pressure of carbon dioxide is 3MPa.
In the present embodiment, the weight ratio of the sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini is 2：1：
1：1.
Embodiment 2：
A kind of preparation method and preparation method thereof of high-purity phosphorus pentachloride, includes the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature is controlled at 120 DEG C, and chlorine is passed through from reactor bottom, until to material in reactor by liquid phase
Become solid crystalline completely, stop leading to chlorine, crystal is made, it is spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 170 DEG C, is made
It obtains coarse crystal and stands 20min completely after by heat sublimation；Then pumping process is carried out, it is using air pump that the gas in heating tank is complete
It is pumped into dustless tank, gas filters before entering dustless tank by filter, impurity trapped, then carries out cooling place to dustless tank
Reason so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
In the present embodiment, filter is heated to 165 DEG C and keeps the temperature until at pumping when the pumping process
Reason terminates.
In the present embodiment, the physical dryness agent is sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini
Mixture.
In the present embodiment, the vaporization process the specific steps are liquid chlorine and liquid carbon dioxide are respectively fed to hot friendship
In heat exchanger, heating water bath is used outside heat exchanger, it is 50 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide are abundant
Vaporization.
In the present embodiment, when the chlorination reaction, the mixing speed of the agitating shaft of reaction kettle is 50r/min, until arriving
Until material becomes solid crystalline completely by liquid phase.
In the present embodiment, in the purge, the purging pressure of carbon dioxide is 6MPa.
In the present embodiment, the weight ratio of the sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini is 2：1：
1：1.
Embodiment 3：
A kind of preparation method and preparation method thereof of high-purity phosphorus pentachloride, includes the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature is controlled at 115 DEG C, and chlorine is passed through from reactor bottom, until to material in reactor by liquid phase
Become solid crystalline completely, stop leading to chlorine, crystal is made, it is spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 165 DEG C, is made
It obtains coarse crystal and stands 20min completely after by heat sublimation；Then pumping process is carried out, it is using air pump that the gas in heating tank is complete
It is pumped into dustless tank, gas filters before entering dustless tank by filter, impurity trapped, then carries out cooling place to dustless tank
Reason so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
In the present embodiment, filter is heated to 165 DEG C and keeps the temperature until at pumping when the pumping process
Reason terminates.
In the present embodiment, the physical dryness agent is sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini
Mixture.
In the present embodiment, the vaporization process the specific steps are liquid chlorine and liquid carbon dioxide are respectively fed to hot friendship
In heat exchanger, heating water bath is used outside heat exchanger, it is 45 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide are abundant
Vaporization.
In the present embodiment, when the chlorination reaction, the mixing speed of the agitating shaft of reaction kettle is 45r/min, until arriving
Until material becomes solid crystalline completely by liquid phase.
In the present embodiment, in the purge, the purging pressure of carbon dioxide is 4MPa.
In the present embodiment, the weight ratio of the sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini is 2：1：
1：1.
Embodiment 4
A kind of preparation method and preparation method thereof of high-purity phosphorus pentachloride, includes the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature is controlled at 118 DEG C, and chlorine is passed through from reactor bottom, until to material in reactor by liquid phase
Become solid crystalline completely, stop leading to chlorine, crystal is made, it is spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 170 DEG C, is made
It obtains coarse crystal and stands 20min completely after by heat sublimation；Then pumping process is carried out, it is using air pump that the gas in heating tank is complete
It is pumped into dustless tank, gas filters before entering dustless tank by filter, impurity trapped, then carries out cooling place to dustless tank
Reason so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
In the present embodiment, filter is heated to 165 DEG C and keeps the temperature until at pumping when the pumping process
Reason terminates.
In the present embodiment, the physical dryness agent is sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini
Mixture.
In the present embodiment, the vaporization process the specific steps are liquid chlorine and liquid carbon dioxide are respectively fed to hot friendship
In heat exchanger, heating water bath is used outside heat exchanger, it is 40 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide are abundant
Vaporization.
In the present embodiment, when the chlorination reaction, the mixing speed of the agitating shaft of reaction kettle is 48r/min, until arriving
Until material becomes solid crystalline completely by liquid phase.
In the present embodiment, in the purge, the purging pressure of carbon dioxide is 5MPa.
In the present embodiment, the weight ratio of the sepiolite fibre, bentonite, semen pulicariae shell powder and pollen pini is 2：1：
1：1.
The beneficial effects of the invention are as follows：The beneficial effects of the invention are as follows：Remaining tri-chlorination is eliminated in the production process
Phosphorus, and the characteristics of phosphorus pentachloride is easy by heat sublimation is utilized, phosphorus pentachloride heating is become into gaseous state, is then extracted into again in addition
It is cooling in one dustless, clean tank so that phosphorus pentachloride becomes crystallization again again in this tank, and is also set in whole process
It is equipped with filtration treatment so that phosphorus pentachloride is detached with impurity, effectively raises the purity of phosphorus pentachloride.
The above description is merely a specific embodiment, but scope of protection of the present invention is not limited thereto, any
The change or replacement expected without creative work should all be covered within the scope of the present invention.
Claims (7)
1. a kind of preparation method of high-purity phosphorus pentachloride, which is characterized in that include the following steps：
1）Liquid chlorine and liquid carbon dioxide are sent into drying tower A and drying tower containing physical dryness agent by closed conduit respectively
In B, the moisture in liquid chlorine and liquid carbon dioxide is sloughed respectively using physical dryness agent, dry liquid chlorine and liquid dioxy is made
Change carbon, it is spare；
2）Liquid chlorine and liquid carbon dioxide are vaporized processing respectively so that liquid chlorine and liquid carbon dioxide become gaseous state, and
It is stored in two surge tanks respectively, chlorine and carbon dioxide is made, it is spare；
3）The phosphorus trichloride of liquid is added in reaction kettle, then by step 2）Chlorine obtained, which is passed into reaction kettle, carries out chlorine
Change reaction, wherein reaction temperature control at 110-120 DEG C, chlorine is passed through from reactor bottom, until to material in reactor by
Liquid phase becomes solid crystalline completely, stops leading to chlorine, and crystal is made, spare；
4）By step 3）Crystal obtained is poured into filter bag, then uses step 2）Carbon dioxide obtained is in dustless ring
Purge is carried out in border, the phosphorus trichloride remained on crystal is removed, and coarse crystal is made；
5）By step 4）Coarse crystal obtained, which is poured into heating tank, to be heated, and the temperature of heat treatment is 160-170
DEG C so that coarse crystal stands 20min completely after by heat sublimation；Then pumping process is carried out, using air pump by the gas in heating tank
Body is completely withdrawn into dustless tank, and gas filters before entering dustless tank by filter, and impurity trapped then carries out dustless tank
Cooling treatment so that gaseous phosphorus pentachloride becomes solid-state again to get high-purity phosphorus pentachloride again.
2. a kind of preparation method of high-purity phosphorus pentachloride as described in claim 1, it is characterised in that：When the pumping process
Filter is heated to 165 DEG C and keeps the temperature until terminating to pumping process.
3. a kind of preparation method of high-purity phosphorus pentachloride as described in claim 1, it is characterised in that：The physical dryness agent
For sepiolite fibre, the mixture of bentonite, semen pulicariae shell powder and pollen pini.
4. a kind of preparation method of high-purity phosphorus pentachloride as described in claim 1, which is characterized in that the vaporization process
The specific steps are liquid chlorine and liquid carbon dioxide to be respectively fed in the hot device of heat exchange, heating water bath is used outside heat exchanger,
It is 40-50 DEG C to be heated to temperature so that liquid chlorine and liquid carbon dioxide fully vaporize.
5. a kind of preparation method of high-purity phosphorus pentachloride as described in claim 1, it is characterised in that：The chlorination reaction
When, the mixing speed of the agitating shaft of reaction kettle is 40-50r/min, until until material becomes solid crystalline completely by liquid phase.
6. a kind of preparation method of high-purity phosphorus pentachloride as described in claim 1, it is characterised in that：The purge
In, the purging pressure of carbon dioxide is 3-6MPa.
7. a kind of preparation method of high-purity phosphorus pentachloride as claimed in claim 3, it is characterised in that：The sepiolite is fine
Dimension, bentonite, semen pulicariae shell powder and pollen pini weight ratio be 2：1：1：1.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201811022336.2A CN108675274A (en) | 2018-09-04 | 2018-09-04 | A kind of preparation method of high-purity phosphorus pentachloride |
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| CN201811022336.2A CN108675274A (en) | 2018-09-04 | 2018-09-04 | A kind of preparation method of high-purity phosphorus pentachloride |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0035201A1 (en) * | 1980-03-04 | 1981-09-09 | Hoechst Aktiengesellschaft | Process for producing phosphorous pentachloride |
| CN1911791A (en) * | 2006-08-29 | 2007-02-14 | 河北科技大学 | Synthesis method of high purity phosphorus pentachloride |
| CN1923676A (en) * | 2006-08-29 | 2007-03-07 | 河北科技大学 | Reactor for synthesizing phosphorus pentachloride |
| CN102897728A (en) * | 2012-10-12 | 2013-01-30 | 徐州江海源精细化工有限公司 | Method for producing phosphorus pentachloride |
-
2018
- 2018-09-04 CN CN201811022336.2A patent/CN108675274A/en active Pending
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| EP0035201A1 (en) * | 1980-03-04 | 1981-09-09 | Hoechst Aktiengesellschaft | Process for producing phosphorous pentachloride |
| CN1911791A (en) * | 2006-08-29 | 2007-02-14 | 河北科技大学 | Synthesis method of high purity phosphorus pentachloride |
| CN1923676A (en) * | 2006-08-29 | 2007-03-07 | 河北科技大学 | Reactor for synthesizing phosphorus pentachloride |
| CN102897728A (en) * | 2012-10-12 | 2013-01-30 | 徐州江海源精细化工有限公司 | Method for producing phosphorus pentachloride |
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