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Preparation method of flaky phosphorus pentasulfide

A phosphorus pentasulfide and flake technology is applied in the field of preparation of flake phosphorus pentasulfide, which can solve the problems of easy occurrence of high phosphorus compounds, inaccurate ratio of raw materials, reduced product purity, etc., and achieves good product quality, sufficient material reaction, and prolonged reaction time. Effect

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

[0004] The technical problem to be solved by the present invention is: the existing phosphorus pentasulfide production device is simple, and after a large amount of materials enter the reactor, the ratio of raw materials is inaccurate, and high-phosphorus compounds are easy to appear in the generated products, which are difficult to remove and greatly reduce the product purity. The problem of providing a kind of preparation method of flaky phosphorus pentasulfide

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] 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. Cool, crush, and serve.

[0013] The pressure in the reactor is controlled at 150Pa.

[0014] The mass ratio of the sulfur and yellow phosphorus is 2.6:1.

[0015] Both the sulfur and the yellow phosphorus are raw materials with a content of 99.99%.

Embodiment 2

[0017] 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. Cool, crush, and serve.

[0018] The pressure in the reactor is controlled at 100Pa.

[0019] The mass ratio of the sulfur and yellow phosphorus is 2.6:1.

[0020] Both the sulfur and the yellow phosphorus are raw materials with a content of 99.99%.

Embodiment 3

[0022] 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. Cool, crush, and serve.

[0023] The pressure in the reactor is controlled at 200Pa.

[0024] The mass ratio of the sulfur and yellow phosphorus is 2.6:1.

[0025] Both the sulfur and the yellow phosphorus are raw materials with a content of 99.99%.

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Abstract

The invention discloses a preparation method of flaky 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, cooling and crushing to obtain the flaky phosphorus pentasulfide. The pressure in the reaction kettle is controlled to be 100-200Pa, and the mass ratio of the sulfur to the yellow phosphorus is 2.6: 1; according to the method, the tubular reactor is additionally arranged so that the raw material ratio and the reaction time are effectively guaranteed, byproducts are greatly reduced, the quality of finished products is improved, and the method 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 method for preparing flake 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 to c...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/14
CPCC01B25/14C01P2004/20
Inventor 张远见
Owner 阳新县晨光化工有限公司