Preparation method for synthetizing sulfur dichloride through gas phase catalysis

A gas-phase catalytic synthesis of sulfur dichloride and sulfur dichloride technology, applied in the direction of sulfur and halogen compounds, can solve the problems of small content, low content, large amount of three wastes, etc., achieve high conversion rate, reduce environmental pollution, operation simple effect

Active Publication Date: 2014-10-15
湖南海利常德农药化工有限公司
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  • Abstract
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  • Application Information

AI Technical Summary

Problems solved by technology

[0016] 1. Since the reaction of disulfide dichloride 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 dichloride in the traditional process sulfur
The conversion rate of sulfur dichloride produced by the above process is lower than 90%, and the content is lower than 87%.
[0017] 2. Most of the catalysts can be removed by filtration in the traditional process, but some catalysts are still dissolved in the sulfur

Method used

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  • Preparation method for synthetizing sulfur dichloride through gas phase catalysis

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Embodiment 1

[0025] Embodiment 1: Preparation of supported ferric chloride granular activated carbon catalyst

[0026] Add 1000g FeCl to the reactor with reflux device 3 ·6H 2 O, dissolve it with 1200g of absolute ethanol, then add 80g of Φ2mm granular activated carbon, heat and reflux for 30min, cool, filter and dry in the air, place in a muffle furnace at 130-150°C and dry to constant weight to obtain a supported catalyst (FeCl 3 / C).

Embodiment 2

[0027] Embodiment 2: Preparation of sulfur dichloride by continuous gas phase method in fixed-bed catalytic tubular reactor

[0028] With the FeCl that makes in embodiment 1 3 / C 40g of granular catalyst is packed in a jacketed glass tubular reactor with an inner diameter of 20mm, the upper and lower ends of the catalyst are filled with magnetic rings, and the jacket is passed through hot water to raise the temperature to 40-50°C. Control the temperature of the vaporization chamber at 130°C, use chlorine gas as the carrier gas, add 67.5g of disulfur dichloride dropwise into the vaporization chamber, the molar ratio of chlorine gas:disulfur dichloride is 10:1, and control the flow rate of the mixed gas to 63.3ml / min . Chlorine and disulfur dichloride mixed gas are reacted through a fixed bed, and then cooled by a condenser to obtain 103.8 g of sulfur dichloride products, which contain 4.1 g of dissolved chlorine and 3.5 g of disulfur dichloride, which are transferred to storag...

Embodiment 3

[0029] Embodiment 3: Preparation of sulfur dichloride by continuous gas phase method in fixed-bed catalytic tubular reactor

[0030] With the FeCl that makes in embodiment 1 3 / C 40g of granular catalyst is loaded into a jacketed glass tube reactor with an inner diameter of 20mm, the upper and lower ends of the catalyst are filled with magnetic rings, and the jacket is passed through hot water to raise the temperature to 30-40°C. Control the temperature of the vaporization chamber at 130°C, use chlorine gas as the carrier gas, add 67.5g of disulfide dichloride dropwise into the vaporization chamber, the molar ratio of chlorine gas:disulfur dichloride is 9:1, and control the flow rate of the mixed gas to 53ml / min. Chlorine and disulfur dichloride mixed gas react by fixed bed, obtain 104.2g of sulfur dichloride product after condenser cooling again, wherein contain dissolved chlorine 3.8g, disulfur dichloride 2.5g, it is transferred to storage Low-temperature sealed storage in ...

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Abstract

The invention discloses a preparation method for synthetizing sulfur dichloride through gas phase catalysis. Granular activated carbon supported by ferric chloride (FeCl3/C) is taken as a catalyst, disulfur dichloride and chorine are taken as a reaction raw material and a carrier gas, a vaporized gas mixture of the disulfur dichloride and the chorine enters a fixed bed catalysis tubular reactor, the sulfur dichloride is prepared with a continuous gas phase catalysis method, the sulfur dichloride produced through the reaction is cooled by a condenser to be collected, and the excess chlorine is recycled. The sulfur dichloride product obtained with the method is free of catalyst residues, distillation is not required, and the content of sulfur dichloride in the product is higher than 90%. The excess chlorine is recycled. The preparation method is simple to operate, continuous, stable, high in conversion rate and free of waste gas and waste liquor emissions, so that the environmental pollution is reduced.

Description

technical field [0001] The invention relates to a preparation method of sulfur dichloride. Background technique [0002] Sulfur dichloride is an important inorganic chemical product, and its molecular structure is: [0003] Cl-S-Cl [0004] It is widely used in organic synthesis, producing acid anhydrides or chlorides of organic acids, additives for high-pressure lubricants and cutting oils, and processing agents for vegetable oils (such as corn oil and soybean oil). It can also be used as a disinfectant and fungicide. [0005] CN95110380 discloses a synthesis method of sulfur dichloride, which uses sulfur and chlorine to synthesize disulfur dichloride at 30-80°C, and then controls the reaction temperature to 30-80°C to pass chlorine gas into the disulfur dichloride liquid Sulfur dichloride gas is produced in the The reaction rate of this method is slow, and the yield has not been reported. [0006] CN91104832 discloses a synthesis method of sulfur dichloride, which use...

Claims

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Application Information

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IPC IPC(8): C01B17/45
Inventor 阳永强王宇彭勇曾雪云赵东江陈明罗先福
Owner 湖南海利常德农药化工有限公司
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