CN100393614C - Synthesis method of high purity phosphorus pentachloride - Google Patents
Synthesis method of high purity phosphorus pentachloride Download PDFInfo
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- CN100393614C CN100393614C CNB2006100482052A CN200610048205A CN100393614C CN 100393614 C CN100393614 C CN 100393614C CN B2006100482052 A CNB2006100482052 A CN B2006100482052A CN 200610048205 A CN200610048205 A CN 200610048205A CN 100393614 C CN100393614 C CN 100393614C
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Abstract
The present invention relates to synthesis process of high purity phosphorus pentachloride, and features that the synthesis process includes the following steps: 1. the reaction of phosphorus trichloride sprayed downwards and chlorine gas introduced upwards in the equal molar amount as material at 110-130 deg.c to produce solid phosphorus pentachloride; 2. raising the temperature to 150-160 deg.c after finishing reaction and maintaining for 0.5-1.0 hr for solid phosphorus pentachloride to sublime; and 3. lowering the temperature to 40-50 deg.c for phosphorus pentachloride vapor to regelate. The present invention has the advantages of fast reaction speed, high product yield, sectional temperature control for meeting the requirement of vaporizing phosphorus trichloride, synthesizing phosphorus pentachloride, subliming phosphorus pentachloride and regelating phosphorus pentachloride separately, high product purity, environment friendship, etc.
Description
Technical field
The present invention relates to a kind of synthetic method of high purity phosphorus pentachloride, belong to inorganic chemistry synthesis and purification technical field.
Background technology
High purity phosphorus pentachloride is widely used as chlorizating agent, catalyzer, dewatering agent etc. in organic synthesis, be characterized in that reaction is fast, yield is high.Be mainly used in the production of the synthetic and lithium hexafluoro phosphate (lithium cell) of medicine intermediate 7-ACA.Shroff etc. are with PCl
3Vaporization at a certain temperature is then with Cl
2Reaction by a certain percentage, the PCl of generation
5On condenser wall, form the crystal type precipitation, again with PCl
5Particle scrapes off from wall, in confined conditions encapsulation.But the synthetic phosphorus pentachloride of this method directly condenses on the wall, and the product purity that obtains is lower, generally about 96%.
Summary of the invention
The objective of the invention is at the prior art defective, providing a kind of condenses-distils-agglomerative phosphorus pentachloride synthetic method again, improves the purity of phosphorus pentachloride.
The object of the present invention is achieved like this: the synthetic method of this high purity phosphorus pentachloride, and its feature comprises:
A, be the raw material reaction with same mole with phosphorus trichloride and chlorine, from reactor head feed downwards continuously, chlorine feeds from reactor bottom phosphorus trichloride with spray pattern, and control reaction temperature generates solid-state phosphorus pentachloride at 110-130 ℃;
B, reaction are warming up to 150-160 ℃ after finishing, and keep 0.5-1.0 hour, make the phosphorus pentachloride distillation:
C, reduce temperature of reaction to 40-50 ℃, the regelation of phosphorus pentachloride steam.
The synthetic method of described high purity phosphorus pentachloride, temperature of reaction described in steps A, B, the C is by changing circulating water flow control.
The synthetic method of described high purity phosphorus pentachloride, the synthesising reacting time of phosphorus pentachloride described in the steps A 5～6h.
The synthetic method of described high purity phosphorus pentachloride, massfraction≤0.0001% of water in the raw material chlorine of building-up reactions.
The synthetic method of described high purity phosphorus pentachloride, described chlorine carries out drying with the vitriol oil+anhydrous magnesium sulfate.
Synthetic method technical progress effect provided by the invention shows, phosphorus trichloride by reactor head through the spraying gun feed, chlorine is by the reactor bottom feed, building-up reactions is carried out with gas-gas convection type, increased probability of collision and contact area between the reactant, the reaction carry out rapidlyer, complete, the yield height, both do not had the chlorine parcel in the product, it is residual also not have phosphorus trichloride; Reaction process adopts stage temperature control, has satisfied respectively that phosphorus trichloride vaporization, phosphorus pentachloride are synthetic, phosphorus pentachloride distillation and agglomerative needs, and product purity effectively improves; Remaining chlorine entered the absorption of sodium hydroxide absorption tower after reaction was finished.Whole piece technology has guaranteed high-level efficiency, high quality, safety, the environmental protection of building-up reactions, and very high theory and practical value are arranged.
Description of drawings
Fig. 1: high purity phosphorus pentachloride synthesis technique flow process
Embodiment
The present invention is a raw material with phosphorus trichloride and chlorine, the massfraction of phosphorus trichloride 〉=99.99%, and the massfraction of water≤0.0001% in the chlorine, chlorine carries out drying with the vitriol oil+anhydrous magnesium sulfate.Phosphorus trichloride and chlorine with etc. the mole mode charging in 1: 1, Cl
2Enter PCl by reactor bottom
3With under the vaporific spray, the about 0.3h of feed time, the feed rate of phosphorus trichloride are 60～70kg/h by reactor head, ON cycle water simultaneously, and control reaction temperature is at 110-130 ℃, PCl
3After chlorine contacted, reaction generated phosphorus pentachloride rapidly, and emits reaction heat, the vaporization of phosphorus trichloride droplet, and reaction is carried out with gas-gas convection type, and the solid-state phosphorus pentachloride of generation condenses on the reactor wall.About 5～the 6h of phosphorus pentachloride generated time after reaction is finished, reduces circulating water flow, makes reactor temperature rise to 150～160 ℃ and kept 0.5-1.0 hour; Phosphorus pentachloride distils under this temperature, is further purified.Improve circulating water flow again, reactor temperature is slowly reduced, reduce to 40～50 ℃ at last, guarantee that the phosphorus pentachloride crystallization after the distillation is complete, the phosphorus pentachloride devaporation that distillation produces, attached on the reactor wall, the about 0.5h of phosphorus pentachloride crystallization time.After reaction is finished, collect, peel off a little, will come off smoothly, enter storage bin, can not cause any infringement reactor through discharge port attached to the phosphorus pentachloride on the reactor wall, check, encapsulation obtains high purity phosphorus pentachloride, purity＞99.5%.Remaining chlorine enters the sodium hydroxide absorption tower, impurity at the bottom of the removing still.
Listed examples of the present invention is intended to further illustrate condenses-distils-synthetic method of the high purity phosphorus pentachloride of condensing again, and protection scope of the present invention is not constituted any restriction.All can obtain the high purity phosphorus pentachloride product with the embodiment of the invention with via claims of the present invention.
Claims (4)
1. the synthetic method of a phosphorus pentachloride, its feature comprises:
A, be the raw material reaction with same mole with the chlorine of massfraction≤0.0001% of water in the phosphorus trichloride of massfraction 〉=99.99% and the chlorine, phosphorus trichloride with spray pattern from the continuous downwards feed of reactor head, chlorine feeds from reactor bottom, control reaction temperature generates solid-state phosphorus pentachloride at 110-130 ℃;
B, reaction are warming up to 150-160 ℃ after finishing, and keep 0.5-1.0 hour, make the phosphorus pentachloride distillation;
C, reduce temperature of reaction to 40-50 ℃, the regelation of phosphorus pentachloride steam.
2. according to the synthetic method of the described phosphorus pentachloride of claim 1, it is characterized in that: temperature of reaction described in steps A, B and the C is by changing circulating water flow control.
3. according to the synthetic method of the described phosphorus pentachloride of claim 1, it is characterized in that: it is characterized in that: described chlorine carries out drying with the vitriol oil+anhydrous magnesium sulfate.
4. according to the synthetic method of the described phosphorus pentachloride of claim 1, it is characterized in that: the synthesising reacting time of phosphorus pentachloride described in the steps A 5～6h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100482052A CN100393614C (en) | 2006-08-29 | 2006-08-29 | Synthesis method of high purity phosphorus pentachloride |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2006100482052A CN100393614C (en) | 2006-08-29 | 2006-08-29 | Synthesis method of high purity phosphorus pentachloride |
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| Publication Number | Publication Date |
|---|---|
| CN1911791A CN1911791A (en) | 2007-02-14 |
| CN100393614C true CN100393614C (en) | 2008-06-11 |
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| CNB2006100482052A Expired - Fee Related CN100393614C (en) | 2006-08-29 | 2006-08-29 | Synthesis method of high purity phosphorus pentachloride |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102583301A (en) * | 2011-01-18 | 2012-07-18 | 孟永 | Preparation method of lithium hexafluorophosphate |
| CN102757027B (en) * | 2012-06-12 | 2014-07-16 | 陕西延长石油集团氟硅化工有限公司 | System and method for preparing high-purity phosphorus pentafluoride |
| CN102897728B (en) * | 2012-10-12 | 2014-10-29 | 徐州江海源精细化工有限公司 | Method for producing phosphorus pentachloride |
| CN108675274A (en) * | 2018-09-04 | 2018-10-19 | 宿州汉泰化工有限公司 | A kind of preparation method of high-purity phosphorus pentachloride |
| CN108793112A (en) * | 2018-09-04 | 2018-11-13 | 宿州汉泰化工有限公司 | A kind of preparation method of phosphorus pentachloride |
| CN112919439B (en) * | 2021-03-10 | 2023-03-21 | 焦作多氟多实业集团有限公司 | Method and device for continuously preparing high-purity 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 |
| CN116139606A (en) * | 2023-03-30 | 2023-05-23 | 徐州宏达新能源科技有限公司 | Device with high-efficient tail gas treatment capacity is used in phosphorus pentachloride production |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3995013A (en) * | 1974-01-03 | 1976-11-30 | Produits Chimiques Ugine Kuhlmann | Process for the preparation of phosphorus pentachloride |
| US4335085A (en) * | 1980-03-04 | 1982-06-15 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorus pentachloride |
| JPH0354106A (en) * | 1989-07-20 | 1991-03-08 | Nippon Soda Co Ltd | Production of phosphorus pentachloride |
| JPH09301707A (en) * | 1996-05-08 | 1997-11-25 | Nippon Chem Ind Co Ltd | Granular phosphorus pentachloride and its production |
-
2006
- 2006-08-29 CN CNB2006100482052A patent/CN100393614C/en not_active Expired - Fee Related
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3995013A (en) * | 1974-01-03 | 1976-11-30 | Produits Chimiques Ugine Kuhlmann | Process for the preparation of phosphorus pentachloride |
| US4335085A (en) * | 1980-03-04 | 1982-06-15 | Hoechst Aktiengesellschaft | Process for the preparation of phosphorus pentachloride |
| JPH0354106A (en) * | 1989-07-20 | 1991-03-08 | Nippon Soda Co Ltd | Production of phosphorus pentachloride |
| JPH09301707A (en) * | 1996-05-08 | 1997-11-25 | Nippon Chem Ind Co Ltd | Granular phosphorus pentachloride and its production |
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| CN1911791A (en) | 2007-02-14 |
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Granted publication date: 20080611 Termination date: 20090929 |