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Synthesis method of high purity phosphorus pentachloride

A technology of phosphorus pentachloride and synthesis method, applied in the direction of phosphorus halide/oxyhalide, etc., can solve the problem of low product purity, and achieve the effects of high yield, improved product purity, high theoretical and practical value

Inactive Publication Date: 2008-06-11
HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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Problems solved by technology

But this method synthesizes phosphorus pentachloride to directly condense on the vessel wall, and the product purity obtained is relatively low, generally around 96%.

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  • Synthesis method of high purity phosphorus pentachloride

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Embodiment Construction

[0014] The invention uses phosphorus trichloride and chlorine gas as raw materials, the mass fraction of phosphorus trichloride is ≥99.99%, the mass fraction of water in chlorine gas is ≤0.0001%, and the chlorine gas is dried with concentrated sulfuric acid+anhydrous magnesium sulfate. Phosphorus trichloride and chlorine are fed in an equimolar 1:1 manner, Cl 2 Entered from the bottom of the reactor, PCl 3 Spray down from the top of the reactor in mist form, the feeding time is about 0.3h, the feeding rate of phosphorus trichloride is 60-70kg / h, and the circulating water is turned on at the same time, the reaction temperature is controlled at 110-130°C, PCl 3 After contacting with chlorine gas, it reacts rapidly to generate phosphorus pentachloride, and releases the reaction heat, the phosphorus trichloride mist is vaporized, and the reaction is carried out by gas-gas convection, and the solid phosphorus pentachloride condenses on the inner wall of the reactor. The synthesis ...

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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 [0001] The invention relates to a method for synthesizing high-purity phosphorus pentachloride, which belongs to the technical field of inorganic chemical synthesis and refining. Background technique [0002] High-purity phosphorus pentachloride is widely used as chlorinating agent, catalyst, dehydrating agent, etc. in organic synthesis, and is characterized by fast reaction and high yield. It is mainly used in the synthesis of pharmaceutical intermediate 7-ACA and the production of lithium hexafluorophosphate (lithium battery). Shroff et al. PCl 3 Vaporize at a certain temperature, and then react with Cl 2 According to a certain proportion of reaction, the generated PCl 5 A crystalline precipitate forms on the wall of the condenser, and the PCl 5 Particles are scraped off the walls of the container and packaged under airtight conditions. However, the synthesis of phosphorus pentachloride by this method is directly condensed on the wall of the vessel, an...

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B25/10
Inventor 魏福祥任清亮王金梅
Owner HEBEI UNIVERSITY OF SCIENCE AND TECHNOLOGY
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