Preparation method and preparation device of sulfur dichloride

A sulfur dichloride and preparation device technology, which is applied in the direction of sulfur dichloride, sulfur and halogen compounds, etc., can solve the problems of large amount of three wastes, affecting product quality, and high requirements for reaction equipment, so as to improve yield and quality, and suppress Reverse reaction, simple operation effect

Active Publication Date: 2019-01-04
湖南海利常德农药化工有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This process has the following three disadvantages: one is that sulfur monochloride needs to be completely gasified, which requires higher requirements for reaction equipment; the other is that the molar ratio of chlorine gas to sulfur monochloride is 5:10-1, and the consumption of chlorine gas per pass is large; Third, since the catalytic reaction temperature is 30-50°C, the sulfur dichloride produced is liquid, and the active ingredient FeCl in the catalyst is 3 There will be a small amount dissolved in liquid sulfur dichloride, affecting the purity of the product
[0011] 1. Since the reaction of sulfur monochloride to obtain sulfur dichloride is a reversible reaction, the reaction is easy to proceed in the direction of the reverse reaction when the chlorine gas is not too much, so it is difficult to achieve high conversion rate and high content of sulfur dichloride in the traditional process
[0012] 2. Most of the catalysts can be removed by filtration in the traditional process, but some catalysts are still dissolved in the sulfur dichloride product, which affects the quality of the product, and the catalyst needs to be separated by distillation
However, a certain amount of phosphorus trichloride (or phosphorus pentachloride, etc.) will be contained in the still liquid after distillation. Under the condition that there is a stabilizer, the still liquid can no longer react with chlorine gas, causing the still liquid to be unable to be recycled. , can only be treated as waste liquid, and the amount of three wastes is large
[0014] 4. The content of sulfur dichloride product distilled by traditional technology is less than 85%

Method used

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  • Preparation method and preparation device of sulfur dichloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] Add 110.00 g (1.63 mol) of sulfur monochloride to the reaction liquid kettle 1, put 40 g of silicon dioxide with a particle diameter of 2 mm into a catalytic reaction tube 31 with an inner diameter of 20 mm, and feed a 65°C liquid into the heating tube 32 to keep it warm. Reactor 1 was heated to 120°C and then chlorine gas was introduced into it. Reactor 1 was maintained at this temperature for 6 hours and then the chlorine was stopped. A total of 88.00 g (1.24 mol) of chlorine was used. The gas phase at the top of the catalytic reactor 3 was condensed by the condenser 4 to obtain 160.93 g of sulfur dichloride product, the product content was 97%, and the product yield was 93%. The uncondensed gas can be recycled after being collected at the gas outlet 41 .

Embodiment 2

[0041] Add 110.00 g (1.63 mol) of sulfur monochloride to the reaction liquid kettle 1, put 40 g of silicon dioxide with a particle diameter of 5 mm into a catalytic reaction tube 31 with an inner diameter of 20 mm, and feed a 65°C liquid into the heating tube 32 Circulating heat preservation, the reaction kettle 1 was heated to 110°C and chlorine gas was introduced, and the reaction kettle 1 was maintained at this temperature for 14 hours before the chlorine flow was stopped, and a total of 88.00 g (1.24 mol) of chlorine was used. The gas phase at the top of the catalytic reactor 3 was condensed by the condenser 4 to obtain 160.86 g of sulfur dichloride product, the product content was 96%, and the product yield was 92%. The uncondensed gas can be recycled after being collected at the gas outlet 41 .

Embodiment 3

[0043] Add 110 g (1.63 mol) of sulfur monochloride to the reaction liquid kettle 1, put 70 g of silicon dioxide with a particle diameter of 3 mm into a catalytic reaction tube 31 with an inner diameter of 20 mm, and feed a 60°C liquid into the heating tube 32 Circulate heat preservation, heat the reaction solution kettle 1 to 90°C, and then pass chlorine gas, stop the chlorine flow after 13 hours of reaction, and share 115.70 g (1.63 mol) of chlorine. The gas phase at the top of the catalytic reactor 3 was condensed by the condenser 4 to obtain 157.58 g of sulfur dichloride product, the product content was 98%, and the product yield was 92%. The uncondensed gas can be recycled after being collected at the gas outlet 41 .

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Abstract

The invention discloses a sulfur dichloride preparation method and preparation device. The preparation method comprises the following steps: carrying out synthesis reaction on sulfur monochloride and chlorine gas as raw materials at a temperature of 60 DEG C to 120 DEG C to obtain a gaseous mixture, loading the obtained gaseous mixture into a catalytic reactor filled with silicon oxide, carrying out catalytic reaction at 60 DEG C to 90 DEG C to obtain a product, condensing the obtained product and collecting the same so as to obtain liquid sulfur dichloride. The preparation device comprises a reaction liquid kettle, the catalytic reactor, a condenser and a receiver kettle, which are communicated with each other in sequence, and the reaction kettle is provided with an air tube, the catalytic reactor comprises a catalytic reaction tube and a heating tube sleeving the catalytic reaction tube, the ends of the catalytic reaction tube are open, one end of the catalytic reaction tube is connected with the reaction liquid kettle, and the other end is connected with the condenser; one end of the heating pipe is provided with a heating medium inlet and the other end is provided with a heating medium outlet. The preparation method has the advantages of simple process, no catalyst residue, no distillation, high product purity and high yield and the like. The device is simple, continuous and stable to operate, and no waste is generated.

Description

technical field [0001] The invention belongs to the technical field of preparation of inorganic chemical products, and in particular relates to a preparation method and a preparation device of sulfur dichloride. Background technique [0002] Sulfur dichloride is an important inorganic chemical product, and its molecular structure is SCl 2 , Widely used in organic synthesis, manufacture of anhydrides or oxides of organic acids, high-pressure lubricants and additives for cutting poker, processing agents for vegetable oils (such as corn oil, soybean oil). It can also be used as a disinfectant and fungicide. [0003] CN95110380 discloses a synthesis method of sulfur dichloride, which uses sulfur and chlorine gas to synthesize sulfur monochloride at 30-80°C, and then controls the reaction temperature at 30-80°C to pass chlorine gas into sulfur monochloride liquid to obtain Sulfur dichloride gas. The reaction rate of this method is slow, and the yield has not been reported. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B17/45
CPCC01B17/4546
Inventor 胡志彬曾雪云徐建兵赵东江曾敬陈明
Owner 湖南海利常德农药化工有限公司
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