Method for recycling tail gas during thionyl chloride preparation

A technology for recovery of thionyl chloride and tail gas, which is applied in the direction of sulfur and halogen compounds, can solve the problems of backward technology, complicated process, and increased tail gas volume, and achieve the effect of saving alkali for tail gas absorption and eliminating environmental pollution

Inactive Publication Date: 2013-04-17
SHANDONG KAISHENG NEW MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] (1) Sulfur trioxide method: Phosphorus pentachloride reacts with sulfur trioxide to generate thionyl chloride and phosphorus oxychloride. The process of this route is simple, but the separation of thionyl chloride and phosphorus oxychloride is difficult, and the product is not easy purify
[0005] (2) Chlorosulfonic acid method: use antimony chloride as a catalyst to react sulfur monochloride with chlorine gas and chlorosulfonic acid. This method has complicated process, backward technology, large material consumption and serious pollution
There are two ways to remove the gas dissolved in the liquid, the heating method and the decompression method, and this degassing method, which depends on increasing the temperature of the material so that the gas is released and returned to the thionyl chloride synthesis kettle, will cause some product loss. Under higher pressure, there are more non-condensable gases such as sulfur dioxide dissolved in it, resulting in an increase in the amount of tail gas in the latter production process
For the rectification tail gas, the patent simply mentions that the diaphragm pump is used to return the thionyl chloride synthesis tank for recycling. This process may cause the pressure of the thionyl chloride synthesis tank to gradually increase and the proportion of reaction materials to be unbalanced

Method used

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  • Method for recycling tail gas during thionyl chloride preparation

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Effect test

Embodiment 1

[0046] What this embodiment describes is the method that the gas released during the feeding process from the crude product vulcanization tank 3 to the crude product intermediate tank 4 is transported back to the thionyl chloride synthesis kettle 1 with a liquid ring compressor 5 for recycling, and the produced product is then recycled. After being condensed by the crude product condenser 2, enter the crude product vulcanization tank 3 for recycling, and the specific implementation method is as follows:

[0047] The vaporized chlorine enters the sulfur dichloride synthesis tank after being metered, and the sulfur monochloride from the de-weighting tower tank in the rectification tower 6 (the rectification tower is composed of a de-weighting tower, a dehydrogenation tower and a product tower) After being metered, it also flows into the sulfur dichloride synthesis tank, and chlorine gas and sulfur monochloride react at 83°C at a ratio of 150:0.25 (liquid) to generate sulfur dichl...

Embodiment 2

[0052] What this embodiment describes is in the sulfur oxychloride distillation process, the condensed tail gas is transported back to the method for recycling the thionyl chloride synthesis kettle 1 with a liquid ring compressor 5, and the specific method is as follows:

[0053] In rectification tower 6, the temperature at the bottom of the weight-removing tower is 130°C, the temperature at the top of the tower is 68°C, the reflux ratio is 1:1, and a secondary vulcanization tank is installed at the top of the tower. The rectification liquefaction tail gas condensed by the condenser 8 is pressurized and sent to the thionyl chloride synthesis kettle 1 by a liquid ring compressor 5 . The liquid ring compressor 5 uses sulfur monochloride as the circulating medium, and the frequency conversion controls the pressure inside the tower. The pressure of the weight removal tower in the rectification tower 6 is stable at -200Pa. When adding sulfur to the secondary vulcanization tank 7, th...

Embodiment 3

[0055] What this embodiment describes is the method that after the secondary vulcanization of solid sulfur with a moisture content of 0.48%, the distillation condensed tail gas is recycled to the thionyl chloride synthesis kettle 1 for circular reaction, and the specific method is as follows:

[0056] In the rectifying tower 6, the temperature of the de-weighting tower bottom is 125°C, the temperature at the top of the tower is 71°C, the reflux ratio is 1:1, and a secondary vulcanization tank 7 is installed at the top of the tower. A liquid ring compressor 5 is used to recover the rectification liquefied tail gas under pressure and send it to the thionyl chloride synthesis kettle 1 . The liquid ring compressor 5 uses a mixture of sulfur monochloride and thionyl chloride as the circulating medium, adopts frequency conversion control, and the pressure in the weight removal tower in the rectification tower 6 is stable at -250Pa. The moisture content of the added solid sulfur is 0...

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Abstract

The invention relates to a method for recycling tail gas during thionyl chloride preparation, which belongs to the field of chemical engineering process. The method is that delivering the gas released during the transportation process of thionyl chloride crude product from a crude product vulcanizing tank to a crude product intermediate tank and the gas remained after the rectification and the condensation of the thionyl chloride to a thionyl chloride synthesis kettle for cyclic utilization by using a gas compression conveying machinery. The sulfur dioxide method thionyl chloride manufacturing technology forms a perfect gas phase closed cycle, which enables the yield of thionyl chloride to be above 99 percent, and saves a great amount of tail gas absorption alkali and eliminates environment pollution. The liquid ring type compressor has the advantages that the operation is simple and convenient, the construction cost is low, the maintenance quantity is small and no additional agent is used in the system.

Description

technical field [0001] The invention relates to a method for recovering and utilizing tail gas in the preparation of thionyl chloride, which belongs to the field of chemical technology. Background technique [0002] Thionyl chloride is an important chlorination agent for organic synthesis, such as the chlorination of alcoholic hydroxyl groups, chlorination of carboxylic acids, chlorination of acid anhydrides, chlorine replacement of organic sulfonic acids or nitro compounds. Manufacture of acid chlorides can also be used in ring closure reactions and Beckmann transpositions. (Extracted from the second edition of "Inorganic Salt Industry Handbook", edited by Tianjin Research Institute of Chemical Industry P601) [0003] Commonly used synthetic methods suitable for industrialized production of thionyl chloride have three kinds: [0004] (1) Sulfur trioxide method: Phosphorus pentachloride reacts with sulfur trioxide to generate thionyl chloride and phosphorus oxychloride. Th...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
Inventor 张善民李云永王荣海时亮李志忠
Owner SHANDONG KAISHENG NEW MATERIALS
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