CN103420349A - Production method of phosphorus pentachloride - Google Patents
Production method of phosphorus pentachloride Download PDFInfo
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- CN103420349A CN103420349A CN2012101581578A CN201210158157A CN103420349A CN 103420349 A CN103420349 A CN 103420349A CN 2012101581578 A CN2012101581578 A CN 2012101581578A CN 201210158157 A CN201210158157 A CN 201210158157A CN 103420349 A CN103420349 A CN 103420349A
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- chlorine
- phosphorus
- phosphorus trichloride
- nitrogen
- reaction kettle
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Abstract
The invention discloses a production method of phosphorus pentachloride, and the product belongs to the field of chemical engineering. The production method takes solid phosphorus trichloride, chlorine, nitrogen, and sodium hydroxide water solution as the raw materials, and makes the phosphorus trichloride and chlorine to carry out reactions in a chemical reactor to generate high pure phosphorus pentachloride through the gas-gas way. The production technology has the advantages of universal equipment, simple technology, convenient raw material source, high conversion rate, high product yield, high purity and environment-friendliness. The product is used for preparing various phosphorus-containing compounds such as phosphonitrilic chloride, etc. in the inorganic industry, and preparing various phosphorus-containing compounds such as phosphoryl chloride, etc. in the organic industry, is capable of being used as a chlorinating agent, and can be applied to the industries such as pharmacy, chemical fiber, and the like. High pure phosphorus pentachloride is mainly used as a medical intermediate and for the synthesis of lithium hexafluorophosphate.
Description
Technical field
The invention belongs to chemical field, relate in particular to a kind of method of phosphorus trichloride as the raw material production phosphorus pentachloride of take.
Background technology
Phosphorus pentachloride, molecular formula is PCl5, molecular weight is 208.24, sterling is white, because after placing, decomposed being arranged, be that phosphorus trichloride and chlorine are faint yellow, generally outward appearance is white or talks yellow tetragonal spheroidal xln, density 1.60g/cm3,167 ℃ of fusing points, be dissolved in dithiocarbonic anhydride, tetracol phenixin and Benzoyl chloride, is hydrolyzed into phosphoric acid and hydrogenchloride in damp atmosphere, produce white cigarette and special stimulation is hidden, start distillation while being heated to 160 ℃, and decomposed is arranged, all resolve into chlorine and phosphorus trichloride during to 300 ℃.Phosphorus pentachloride PCl5 is widely used as chlorizating agent, catalyzer, dewatering agent in organic synthesis, and inorganic industry is for producing various P contained compounds, as phosphonitrilic chloride etc.; Organic industry is for producing various P contained compounds as phosphoryl chloride etc., also as chlorizating agent, as oxalyl chloride, succinic chloride and catalyzer etc.; In addition also for industry such as pharmacy, chemical fibres.Highly purified phosphorus pentachloride, be mainly used in the synthetic of medicine intermediate and lithium hexafluoro phosphate.The at present production of phosphorus pentachloride adopts traditional processing technology mostly, and take phosphorus trichloride, chlorine etc. is raw material, first injects a certain amount of liquid phosphorus trichloride in the stirring-type reactor, pass into again chlorine, with gas, liquid way of contact reaction, between this technological reaction thing, contact area is little, and reaction not exclusively, product yield is low, the phosphorus pentachloride generated easily condenses in reactor, forms hard bulk, causes the discharging difficulty, equipment is perishable, damage, and is difficult to produce highly purified phosphorus pentachloride.The defect existed in order to overcome traditional phosphorus pentachloride production technique, the present invention by phosphorus trichloride and chlorine in the mode of gaseous state in reaction kettle for reaction, overcome between the gas, liquid way of contact reactant of traditional technology contact area little, reaction not exclusively, the defect that product yield is low, finally make phosphorus pentachloride.This production technique has uses that general-purpose equipment, technique are simple, raw material sources facilitate the series of advantages such as transformation efficiency is high, product yield is high, purity is high, environmental protection.
Summary of the invention
The problem that the present invention mainly solves is to provide a kind of method of producing phosphorus pentachloride in batches, it is raw material that the method be take by phosphorus trichloride, chlorine, nitrogen, mode by the contact of gas gas in reactor is reacted, its advantage is: use general-purpose equipment, technique is simple, raw material sources are convenient, product yield is high, purity is high, disposable output is large, the raw material of the present invention's use is: solid phosphorus trichloride, chlorine, nitrogen, aqueous sodium hydroxide solution.
The present invention can be achieved through the following technical solutions:
A kind of production method of phosphorus pentachloride, its feature consists of following steps:
(1) phosphorus trichloride of formula ratio is sent into to the phosphorus trichloride spraying gun, send into nitrogen by being arranged at nitrogen inlet on spraying gun, phosphorus trichloride: nitrogen=1-1.2:2-2.2, the phosphorus trichloride that makes to enter in the nitrogen atomization device forms phosphorus trichloride gas under the effect of nitrogen.
(2) by pipeline, phosphorus trichloride gas is sent into to chemical reaction kettle, chlorine is sent into after the chlorine filter device filters and entered gauger by pipeline simultaneously, send into airtight chemical reaction kettle by pipeline after metering, the mol ratio that the amount of controlling chlorine by gauger is controlled phosphorus trichloride gas and chlorine is 1:1-1.2, send into steam by the steam inlet on chemical reaction kettle in the chemical reaction kettle interlayer, reactor temperature is brought up to 90 ℃-100 ℃, make mixed gas hybrid reaction 1.5 hours in still, reaction finishes, generate highly purified phosphorus pentachloride solid and a small amount of remaining chlorine in still.
(3) reaction is discharged a small amount of remaining chlorine after finishing by the outlet on chemical reaction kettle, with aqueous sodium hydroxide solution, absorbs, and the phosphorus pentachloride solid is taken out from the outlet of chemical reaction kettle, after packing, gets product.
The invention has the beneficial effects as follows: a kind of production method of phosphorus pentachloride is provided, and the advantage of this production method is: use general-purpose equipment, technique is simple, raw material sources are convenient, product yield is high, purity is high, disposable output greatly, environmental protection.
Embodiment
Embodiment 1
The phosphorus trichloride of formula ratio is sent into to the phosphorus trichloride spraying gun, by being arranged at nitrogen inlet on spraying gun, send into nitrogen, phosphorus trichloride: nitrogen=1:2, the phosphorus trichloride that makes to enter in the nitrogen atomization device forms phosphorus trichloride gas under the effect of nitrogen, by pipeline, phosphorus trichloride gas is sent into to chemical reaction kettle, chlorine is sent into after the chlorine filter meter filters and entered gauger by pipeline simultaneously, send into airtight chemical reaction kettle by pipeline after metering, the mol ratio that the amount of controlling chlorine by gauger is controlled phosphorus trichloride gas and chlorine is 1:1, send into steam by the steam inlet on chemical reaction kettle in the chemical reaction kettle interlayer, reactor temperature is brought up to 90 ℃, make mixed gas hybrid reaction 1.5 hours in still, reaction finishes, generate highly purified phosphorus pentachloride solid and a small amount of remaining chlorine in still, after reaction finishes, a small amount of remaining chlorine is discharged by the outlet on chemical reaction kettle, absorb with aqueous sodium hydroxide solution, the phosphorus pentachloride solid is taken out from the outlet of chemical reaction kettle, get product after packing.
Embodiment 2
The phosphorus trichloride of formula ratio is sent into to the phosphorus trichloride spraying gun, by being arranged at nitrogen inlet on spraying gun, send into nitrogen, phosphorus trichloride: nitrogen=1.1:2.1, the phosphorus trichloride that makes to enter in the nitrogen atomization device forms phosphorus trichloride gas under the effect of nitrogen, by pipeline, phosphorus trichloride gas is sent into to chemical reaction kettle, chlorine is sent into after the chlorine filter meter filters and entered gauger by pipeline simultaneously, send into airtight chemical reaction kettle by pipeline after metering, the mol ratio that the amount of controlling chlorine by gauger is controlled phosphorus trichloride gas and chlorine is 1:1.1, send into steam by the steam inlet on chemical reaction kettle in the chemical reaction kettle interlayer, reactor temperature is brought up to 95 ℃, make mixed gas hybrid reaction 1.5 hours in still, reaction finishes, generate highly purified phosphorus pentachloride solid and a small amount of remaining chlorine in still, after reaction finishes, a small amount of remaining chlorine is discharged by the outlet on chemical reaction kettle, absorb with aqueous sodium hydroxide solution, the phosphorus pentachloride solid is taken out from the outlet of chemical reaction kettle, get product after packing.
Embodiment 3
The phosphorus trichloride of formula ratio is sent into to the phosphorus trichloride spraying gun, by being arranged at nitrogen inlet on spraying gun, send into nitrogen, phosphorus trichloride: nitrogen=1.2:2.2, the phosphorus trichloride that makes to enter in the nitrogen atomization device forms phosphorus trichloride gas under the effect of nitrogen, by pipeline, phosphorus trichloride gas is sent into to chemical reaction kettle, chlorine is sent into after the chlorine filter meter filters and entered gauger by pipeline simultaneously, send into airtight chemical reaction kettle by pipeline after metering, the mol ratio that the amount of controlling chlorine by gauger is controlled phosphorus trichloride gas and chlorine is 1:1.2, send into steam by the steam inlet on chemical reaction kettle in the chemical reaction kettle interlayer, reactor temperature is brought up to 100 ℃, make mixed gas hybrid reaction 1.5 hours in still, reaction finishes, generate highly purified phosphorus pentachloride solid and a small amount of remaining chlorine in still, after reaction finishes, a small amount of remaining chlorine is discharged by the outlet on chemical reaction kettle, absorb with aqueous sodium hydroxide solution, the phosphorus pentachloride solid is taken out from the outlet of chemical reaction kettle, get product after packing.
Claims (3)
1. the production method of a phosphorus pentachloride, its composition of raw materials is, comprises:: solid phosphorus trichloride, chlorine, nitrogen, aqueous sodium hydroxide solution, it is characterized in that: step (1) is sent the phosphorus trichloride of formula ratio into the phosphorus trichloride spraying gun, send into nitrogen by being arranged at nitrogen inlet on spraying gun, phosphorus trichloride: nitrogen=1-1.2:2-2.2, the phosphorus trichloride that makes to enter in the nitrogen atomization device forms phosphorus trichloride gas under the effect of nitrogen, step (2) is sent phosphorus trichloride gas into chemical reaction kettle by pipeline, chlorine is sent into after the chlorine filter device filters and entered gauger by pipeline simultaneously, send into airtight chemical reaction kettle by pipeline after metering, the mol ratio that the amount of controlling chlorine by gauger is controlled phosphorus trichloride gas and chlorine is 1:1-1.2, send into steam by the steam inlet on chemical reaction kettle in the chemical reaction kettle interlayer, reactor temperature is brought up to 90 ℃-100 ℃, make mixed gas hybrid reaction 1.5 hours in still, reaction finishes, generate highly purified phosphorus pentachloride solid and a small amount of remaining chlorine in still, after step (3) reaction finishes, a small amount of remaining chlorine is discharged by the outlet on chemical reaction kettle, absorb with aqueous sodium hydroxide solution, the phosphorus pentachloride solid is taken out from the outlet of chemical reaction kettle, get product after packing.
2. the production method of a kind of phosphorus pentachloride according to claim 1, the feature of its step (2) is: the mol ratio of described phosphorus trichloride gas and chlorine is 1:1.1.
3. the production method of a kind of phosphorus pentachloride according to claim 1, the feature of its step (2) is: described reactor interior reaction temperature is 95 ℃.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101581578A CN103420349A (en) | 2012-05-21 | 2012-05-21 | Production method of phosphorus pentachloride |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2012101581578A CN103420349A (en) | 2012-05-21 | 2012-05-21 | Production method of phosphorus pentachloride |
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| CN103420349A true CN103420349A (en) | 2013-12-04 |
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| CN2012101581578A Pending CN103420349A (en) | 2012-05-21 | 2012-05-21 | Production method of phosphorus pentachloride |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147382A (en) * | 2018-03-08 | 2018-06-12 | 江西吉翔医药化工有限公司 | A kind of synthetic method of phosphorus pentachloride |
| CN112919439A (en) * | 2021-03-10 | 2021-06-08 | 多氟多化工股份有限公司 | Method and device for continuously preparing high-purity phosphorus pentachloride |
| CN113104825A (en) * | 2021-04-01 | 2021-07-13 | 多氟多化工股份有限公司 | Preparation method of phosphorus chloride |
-
2012
- 2012-05-21 CN CN2012101581578A patent/CN103420349A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108147382A (en) * | 2018-03-08 | 2018-06-12 | 江西吉翔医药化工有限公司 | A kind of synthetic method of phosphorus pentachloride |
| CN112919439A (en) * | 2021-03-10 | 2021-06-08 | 多氟多化工股份有限公司 | Method and device for continuously preparing high-purity phosphorus pentachloride |
| CN113104825A (en) * | 2021-04-01 | 2021-07-13 | 多氟多化工股份有限公司 | Preparation method of phosphorus chloride |
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Application publication date: 20131204 |