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Preparation method of phosphorus pentasulfide

A technology of phosphorus pentasulfide and yellow phosphorus, which is applied in the field of preparation of phosphorus pentasulfide by the liquid phase method, can solve the problems of low product quality, insufficient purity of the final product, complicated preparation process, etc., and achieve improved product yield, improved thermal stability and Antioxidant, side effect reduction effect

Active Publication Date: 2010-09-29
辽宁瑞兴化学有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] It can be seen that the existing phosphorus pentasulfide preparation process has defects such as complicated preparation process or low quality of the obtained product.
At present, the relatively advanced production process of phosphorus pentasulfide is the liquid phase method provided by Italmatch, but the obtained phosphorus pentasulfide still contains 0.155-0.175% by-product (P 4 S 7 ,P 4 S 9 etc.), the purity of the final product is not high enough

Method used

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  • Preparation method of phosphorus pentasulfide
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  • Preparation method of phosphorus pentasulfide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-6

[0031] Embodiment 1-6: the comparison of feeding mode change

[0032] Table 1

[0033]

[0034] As can be seen from Table 1, under substantially the same reaction conditions, the feeding methods are different and the product yields are different. Adopting the nozzle type feeding of the present invention can improve the product yield by 7-8% compared with the straight pipe feeding.

[0035] In Examples 7-18, the nozzle-type feeding method was adopted, and the experimental results under the control of different process parameters were compared.

[0036] The results are shown in Table 2 and Table 3.

[0037] Table 2

[0038] parameter control

[0039] table 3

[0040] parameter control

[0041] Reactor liquid level%

[0042] Find out by table 2 and table 3, the product of higher purity has been obtained in the scope of the selected reaction conditions and distillation conditions of the present invention, and product purity can be up to more tha...

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Abstract

The invention relates to a preparation method of phosphorus pentasulfide by a liquid phase method, and the preparation method comprises the following steps: 1) molten sulphur and molten yellow phosphorus are continuously conveyed into a reaction kettle according to stoichiometric proportion, liquid phase reaction is carried out under stirring, the constant reaction temperature in the reaction kettle is 410-430 DEG C, the constant reaction pressure is 17-21 millibars (gauge pressure, micro positive pressure), and the pressure is generated by introduced nitrogen; and 2) after the reaction, the materials are continuously pumped into a distillation kettle, reduced pressure distillation is carried out in the distillation kettle by utilizing reaction heat, the constant distillation temperature is 390-395 DEG C, and the constant distillation vacuum degree is 80-95 millibars (absolute pressure). By using the preparation method, purer products can be obtained, and the energy consumption is reduced.

Description

technical field [0001] The invention relates to a preparation method for producing phosphorus pentasulfide by adopting a liquid phase method, in particular to the improvement of the reaction and distillation process of phosphorus pentasulfide, and also to the improvement of the feeding method. Background technique [0002] Phosphorus pentasulfide P 2 S 5 (Also known as tetraphosphorus decasulfide P 4 S 10 ) is a light yellow and yellow-green crystalline substance, has an odor similar to hydrogen sulfide, and has strong hygroscopicity. Additives, can be used in the preparation of various sulfur- and phosphorus-containing compounds in organic synthesis, and can also be used to prepare medicines. In recent years, with the understanding of the toxicity of pesticide residues, the amount of organophosphorus pesticides is decreasing year by year due to their inherent characteristics. On the contrary, with the development of industries such as automobiles, petroleum, and medicin...

Claims

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Application Information

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IPC IPC(8): C01B25/14
Inventor 李刚
Owner 辽宁瑞兴化学有限公司
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