Method for preparing sulfur dichloride

A technology of sulfur dichloride and disulfide dichloride, applied in chemical instruments and methods, chemical/physical processes, sulfur and halogen compounds, etc., can solve problems such as harm to the health of operators, environmental pollution, and inconvenience in implementation , to achieve the effect of facilitating popularization and application, no environmental pollution, and easy implementation

Inactive Publication Date: 2004-02-11
淄博市新材料研究所
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The raw material consumption of this preparation method is high, the cost of distillation process is high, and the product yield is low, only 70%, and about 30% of the distillation raffinate cannot be used, and the stability of the product is poor, resulting in high impurity content of disulfide dichloride, resulting in the product The purity is low, and what is more serious is that the decomposition of the product during the distillation process will produce harmful gases, endangering the health of the operators, making it inconvenient to implement, and causing serious pollution to the surrounding environment

Method used

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  • Method for preparing sulfur dichloride

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Experimental program
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Effect test

Embodiment 1

[0017] In the preparation method of sulfur dichloride described in the present invention, the molar ratio of chlorine gas to sulfur is 2.05:1. Add sulfur and iron trichloride catalyst corresponding to 0.15% by weight of sulfur dichloride in the reaction kettle, then feed chlorine gas, control the reaction temperature to be 90-100°C, and control the reaction pressure to gauge pressure 0.1-0.15Mpa. Get disulfur dichloride;

[0018] Cool disulfur dichloride to 2-8°C, and feed chlorine gas to the set ventilation rate to produce sulfur dichloride product;

[0019] Add sulfur dichloride ethyl phosphite stabilizer of 0.2% by weight of sulfur dichloride after resting, obtain the finished product of sulfur dichloride with good stability, the purity reaches more than 98%, the storage period can reach 3 months, and the purity is not less than 95%. Easy to store and use.

[0020] Under the completely identical situation of other conditions, only the different stabilizers used for the pr...

Embodiment 2

[0023] In the preparation method of sulfur dichloride described in the present invention, the molar ratio of chlorine gas to sulfur is 2.06:1. Add sulfur and its equivalent iron trichloride catalyst of 0.12% by weight of sulfur dichloride in the reaction kettle, then feed chlorine gas, control the reaction temperature to be 80-90°C, and the reaction pressure to be controlled at a gauge pressure of 0.15-0.18Mpa. Get disulfur dichloride;

[0024] Cool disulfur dichloride to -6~-1°C, and then pass chlorine gas into it to produce sulfur dichloride product;

[0025] After standing still, 0.4% by weight of sulfur dichloride is added as a butyl phosphite stabilizer to obtain a finished product of sulfur dichloride.

Embodiment 3

[0027] In the preparation method of sulfur dichloride described in the present invention, the molar ratio of chlorine gas to sulfur is 2.03:1. Add sulfur and zinc chloride catalyst equivalent to 0.16% by weight of sulfur dichloride in the reaction kettle, then feed chlorine gas, control the reaction temperature to 110-120°C, and control the reaction pressure to a gauge pressure of 0.1-0.12Mpa to obtain Disulfur dichloride;

[0028] Cool disulfur dichloride to -8~-4°C, and then pass chlorine gas into it to produce sulfur dichloride product;

[0029] After resting, 0.5% by weight of sulfur dichloride is added as a dimethyl hydrogen phosphite stabilizer to obtain a finished product of sulfur dichloride.

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Abstract

The present invention relates to chemical synthesis technology. Sulfur dichloride is prepared through gas-solid reaction between chlorine and sulfur and subsequent cooling. During the reaction between chlorine and sulfur, disulfur dichloride is first produced; after the temperature is lowered and more chloride is introduced, sulfur dichloride is then produced; and after the reaction is finished, stabilizer is added to obtain the product. The said process has high sulfur dichloride yield, has stability, high purity over 98 %, low cost, no environment and is suitable for industrial production.

Description

technical field [0001] The invention relates to a new method for preparing sulfur dichloride, belonging to the technical field of chemical synthesis. Background technique [0002] The existing preparation of sulfur dichloride is carried out with chlorine and sulfur as raw materials, and its preparation process adopts the distillation method, that is, sulfur and chlorine gas are reacted under the action of a catalyst, and then the reaction liquid is distilled to obtain fractions It is sulfur dichloride, in order to strengthen product stability and prevent unstable sulfur dichloride from decomposing into disulfur dichloride, and then add phosphorus trichloride stabilizer. The raw material consumption of this preparation method is high, the cost of the distillation process is high, and the product yield is low, only 70%, about 30% of the distillation raffinate cannot be utilized, and the stability of the product is poor, resulting in high impurity content of disulfur dichloride...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/128C01B17/45
Inventor 朱永国王文举黄东华
Owner 淄博市新材料研究所
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