Multistage rectification process for high-purity thionyl chloride

A thionyl chloride, high-purity technology, applied in the field of multi-stage rectification of high-purity thionyl chloride, can solve problems such as difficult to obtain high-purity thionyl chloride

Active Publication Date: 2008-10-15
JIANGXI SELON INDAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] However, the purification of thionyl chloride involved in the above methods is all single-stage rectification, and it is difficult to obtain high-purity thionyl chloride above 99.6%.

Method used

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  • Multistage rectification process for high-purity thionyl chloride
  • Multistage rectification process for high-purity thionyl chloride

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] 1. Primary distillation

[0049] Pass 50% thionyl chloride into the first-stage rectification column, the temperature of the tower bottom is 110°C, and 80% of the thionyl chloride is obtained at the top of the tower, and the high boiler S in the bottom of the tower is 2 Cl 2 discharge to storage tanks;

[0050] 2. Secondary distillation

[0051] Pass 80% thionyl chloride into the secondary rectification tower. The process parameters are: the temperature of the tower still is controlled at 78-89°C. When the tower still reaches 3 / 4 of the still liquid level and the temperature reaches 89°C, the tower The high mixture in the still is discharged to the still of the primary distillation tower, and about 98% SOCl is obtained from the top of the tower 2 .

[0052] 3. Three-stage distillation

[0053] 98% SOCl 2 Add to the three-stage rectifying tower still by metering, control the tower still temperature at 78-89 ℃, 72-75 ℃ at the top of the tower, and the pressure at th...

Embodiment 2

[0056] Others are the same as embodiment 1, and the difference is that in this embodiment, the following parameters are selected:

[0057] 1. Primary distillation

[0058] Pass 70% thionyl chloride into the first-stage rectification column, the temperature of the tower bottom is 130°C, and 92% of the thionyl chloride is obtained at the top of the tower, and the high boiler S in the bottom of the tower is 2 Cl 2 discharge to storage tanks;

[0059] 2. Secondary distillation

[0060] Pass 92% thionyl chloride into the secondary rectification tower. The process parameters are: the temperature of the tower bottom is controlled at 78-89°C. The high mixture in the still is discharged to the still of the primary distillation tower, and about 98% SOCl is obtained from the top of the tower 2 .

[0061] 3. Three-stage distillation

[0062] 98% SOCl 2 Add to the three-stage rectifying tower still by metering, control the tower still temperature at 78-89 ℃, 76-80 ℃ at the top of th...

Embodiment 3

[0064] Others are the same as embodiment 1, and the difference is that in this embodiment, the following parameters are selected:

[0065] 1. Primary distillation

[0066] Pass 75% thionyl chloride into the primary distillation column, the temperature of the tower bottom is at 120°C, and 95% of the thionyl chloride is obtained at the top of the tower, and the high boiler S in the bottom of the tower is 2 Cl 2 discharge to storage tanks;

[0067] 2. Secondary distillation

[0068] Pass 95% thionyl chloride into the secondary rectification tower. The process parameters are: the temperature of the tower bottom is controlled at 78-89°C. The high mixture in the tower bottom is discharged to the first-stage rectification tower bottom, and about 99% SOCl is obtained from the top of the tower 2 .

[0069] 3. Three-stage distillation

[0070] 99% SOCl2. is metered into the three-stage rectification tower still, and the temperature of the tower still is controlled at 78-89 ° C, 72...

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Abstract

The invention relates to a multistage distillation method for thionyl chloride with high purity. A crude product of the thionyl chloride with the purity of about 70 percent can be purified to more than 99.6 percent by adopting the multistage purification method by steps.

Description

technical field [0001] The invention relates to a high-purity sulfur oxychloride multi-stage rectification method, through which about 70% of the crude thionyl chloride is purified to more than 99.6% by adopting multi-stage and step-by-step purification. Background technique [0002] Thionyl chloride is soluble in benzene, chloroform and carbon tetrachloride, decomposes in water to generate sulfurous acid and hydrogen chloride, and decomposes to generate chlorine gas, sulfur dioxide and sulfur monochloride when heated to 140 degrees, and the chlorine atom of thionyl chloride replaces hydroxyl and mercapto It has a strong ability and can sometimes replace sulfur dioxide, oxygen or hydrogen. It can react with organic compounds such as phenols or alcohols with hydroxyl groups to generate corresponding chlorides, react with sulfonic acids to generate sulfonyl chlorides, and react with Grignard reagents to generate corresponding sub- Sulfone compounds, etc. Thionyl chloride is v...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B17/45
Inventor 汪国清汪新泉戴恒文潘英曙李世群郑小辉刘朔
Owner JIANGXI SELON INDAL
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