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Preparation method of powdery phosphorus pentasulfide

A powdery phosphorus pentasulfide technology, which is applied in the field of powdery phosphorus pentasulfide preparation, can solve the problems of unfriendly environment and operators, low product purity, inaccurate proportioning, etc., so as to avoid the harm to the environment and human body, high content, The effect of prolonging the reaction time

Inactive Publication Date: 2021-05-28
阳新县晨光化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved by the present invention is: when currently preparing phosphorus pentasulfide, the proportion of materials in the reactor is not accurate, resulting in low product purity, and during the pulverization process of flake phosphorus pentasulfide, the flying dust is unfriendly to the environment and operators. And it is easy to cause the problem of combustion accident, and a kind of preparation method of powdery phosphorus pentasulfide is provided

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] A preparation method of flaky phosphorus pentasulfide, comprising the following steps: first heat sulfur and yellow phosphorus with steam, enter the sulfur melting tank and phosphorus melting tank for liquefaction, and then enter the tubular reactor through a metering liquid phase pump to control the reaction The temperature is 440°C, and then enters the reaction kettle through the tubular reactor, and the reaction temperature is controlled in the reaction kettle to be 460°C, and the reaction temperature is kept at 0.6 hours, and it is carried out under nitrogen atmosphere. Cooling; put the flaky phosphorus pentasulfide into the grinding equipment, add carbon tetrachloride protective solvent to submerge the flaky phosphorus pentasulfide, grind for 1.5 hours, and vacuum filter to obtain powdery phosphorus pentasulfide, carbon tetrachloride is recovered and used mechanically.

[0014] The pressure in the reactor is controlled at 150Pa.

[0015] The mass ratio of the sulfu...

Embodiment 2

[0018] A preparation method of flaky phosphorus pentasulfide, comprising the following steps: first heat sulfur and yellow phosphorus with steam, enter the sulfur melting tank and phosphorus melting tank for liquefaction, and then enter the tubular reactor through a metering liquid phase pump to control the reaction The temperature is 400°C, and then enters the reactor through the tubular reactor, and the reaction temperature is controlled at 480°C in the reactor, and it is kept for 0.5 hours, and it is carried out under a nitrogen atmosphere. Cooling; put the flaky phosphorus pentasulfide into the grinding equipment, add carbon tetrachloride protective solvent to submerge the flake phosphorus pentasulfide, grind for 1 hour, and vacuum filter to obtain powdery phosphorus pentasulfide, which is recycled by carbon tetrachloride.

[0019] The pressure in the reactor is controlled at 100Pa.

[0020] The mass ratio of the sulfur and yellow phosphorus is 2.6:1.

[0021] Both the su...

Embodiment 3

[0023] A preparation method of flaky phosphorus pentasulfide, comprising the following steps: first heat sulfur and yellow phosphorus with steam, enter the sulfur melting tank and phosphorus melting tank for liquefaction, and then enter the tubular reactor through a metering liquid phase pump to control the reaction The temperature is 480°C, and then it enters the reactor through the tubular reactor, and the reaction temperature is controlled in the reactor at 440°C, and it stays for 1 hour, and it is carried out under a nitrogen atmosphere. Cooling; put the flaky phosphorus pentasulfide into the grinding equipment, add carbon tetrachloride protective solvent to submerge the flaky phosphorus pentasulfide, grind for 2 hours, and vacuum filter to obtain powdery phosphorus pentasulfide, carbon tetrachloride is recovered and used mechanically.

[0024] The pressure in the reactor is controlled at 200Pa.

[0025] The mass ratio of the sulfur and yellow phosphorus is 2.6:1.

[0026...

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PUM

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Abstract

The invention discloses a preparation method of powdery phosphorus pentasulfide. The preparation method comprises the following steps: firstly, carrying out hot melting on sulfur and yellow phosphorus by using steam, liquefying in a sulfur melting tank and a phosphorus melting tank, then entering a tubular reactor through a metering liquid phase pump, controlling the reaction temperature at 400-480 DEG C, entering a reaction kettle through the tubular reactor, controlling the reaction temperature in a reaction kettle to be 440-480 DEG C, staying for 0.5-1 hour, carrying out reaction in a nitrogen atmosphere, and after the reaction is completed, pressing into flaky phosphorus pentasulfide through a 200-300 DEG C roller, and cooling; putting flaky phosphorus pentasulfide into grinding equipment, adding a carbon tetrachloride protective solvent to submerge the flaky phosphorus pentasulfide, grinding for 1-2 hours, carrying out vacuum filtration to obtain powdery phosphorus pentasulfide, and recycling carbon tetrachloride; through reasonable process design, the preparation method of the powdery phosphorus pentasulfide, which is high in phosphorus pentasulfide content and small in environmental pollution, is provided, and is suitable for wide popularization and application.

Description

technical field [0001] The invention relates to the technical field of preparing phosphorus pentasulfide, in particular to a preparation method of powdery phosphorus pentasulfide. Background technique [0002] Phosphorus pentasulfide is an important raw material for the synthesis of pesticides. It reacts with alcohol to obtain an important phosphorus-containing intermediate "sulfide", which can further synthesize a variety of dithiophosphate pesticides, such as dimethoate, phorate, malathion, etc. ; From "sulfide" chlorination, another important phosphorus-containing intermediate "chloride" can be obtained, and a variety of phosphorothioate pesticides can be synthesized, such as fenitrothion, phoxim, diazinon, etc. , In addition, it is also used as non-ferrous metal beneficiation agent, advanced lubricating oil additive, etc., as well as for match manufacturing, pharmaceutical products and rubber vulcanization auxiliary agent. [0003] Phosphorus and sulfur are very prone t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/14
CPCC01B25/14
Inventor 张远见
Owner 阳新县晨光化工有限公司