Process for producing dimethyl sulfone by double-column rectification

A technology of dimethyl sulfone and double-column rectification is applied in the field of double-column rectification to produce dimethyl sulfone, and can solve the problems such as difficulty in realizing the improvement of the purity of dimethyl sulfone.

Active Publication Date: 2021-09-07
新疆兴发化工有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the good miscibility of dimethyl sulfone, dimethyl sulfoxide and water, it is difficult to further improve the purity of dimethyl sulfone in the operation mode of extracting different fractions from different positions in the single column purification mode

Method used

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  • Process for producing dimethyl sulfone by double-column rectification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] A device for producing dimethyl sulfone by rectification with two towers, the feed pipe 7 is connected to the middle part of the mother rectification tower 1, the bottom of the mother rectification tower 1 is connected to the reboiler 3, and the reboiler 3 is connected to the bottom of the sub rectification tower 2 , the top of the sub-distillation tower 2 is connected to the atomizing crystallizer 4, the atomizing crystallizer 4 is connected to the storage tank one 8, and the bottom of the atomizing crystallizer 4 and the storage tank one 8 are connected to the product area through pipelines respectively, and the one way Connected to sub-rectification column 2 upper part.

[0019] The top of the mother rectification tower 1 is connected to the condenser 6 , and the bottom of the condenser 6 is connected to the upper part of the mother rectification tower 1 .

[0020] The condenser 6 is connected to the second storage tank 9, and the second storage tank 9 is connected t...

Embodiment 2

[0024] A kind of operation of the process scheme of producing high-purity dimethyl sulfone by utilizing the double-tower rectification principle:

[0025] The fraction to be separated enters the mother tower from the feeding point of the mother tower, and water, dimethyl sulfoxide and a small amount of dimethyl sulfone are extracted from the top of the mother tower;

[0026] Through the control of the reflux ratio, a large amount of high-purity dimethyl sulfone is extracted from the top of the sub-tower; the bottom of the sub-tower adopts continuous or intermittent operation mode to remove the dimethyl sulfone solution with increasing inorganic salt concentration in time; After pretreatment, the overhead distillate from the residual and parent tower returns to the twin towers together with the fraction to be separated, so as to realize the recovery and utilization of dimethyl sulfone. The top fraction of the sub-column is granulated and screened by an atomization crystallizer ...

Embodiment 3

[0028] An operational example of a process scheme for producing high-purity dimethyl sulfone using the principle of double-column rectification:

[0029] When the vacuum degree in the tower reaches above 85KPa, the fraction to be separated (dimethyl sulfone content ≥ 95%, water ≤ 2%, inorganic salt ≤ 2%, dimethyl sulfoxide ≤ 1%) is sent from the mother rectification tower The feed point enters the mother tower, and the temperature at the bottom of the tower is controlled at about 160°C. Since water and dimethyl sulfoxide with low boiling points cannot reach the bottom of the mother rectification tower, they rise directly from the stripping section of the mother rectification tower, entraining A small amount of dimethyl sulfone is extracted from the top of the mother distillation column; dimethyl sulfone and salts with higher boiling points enter the sub-rectification column through the reboiler, and the temperature at the top of the column is maintained by controlling the reflu...

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Abstract

The invention provides a device for producing dimethyl sulfone by double-tower rectification. The feed pipe is connected to the middle part of the mother rectification tower, the bottom of the mother rectification tower is connected to the reboiler, the reboiler is connected to the bottom of the sub-rectification tower, and the sub-rectification tower is connected to the bottom of the sub-rectification tower. The top of the distillation tower is connected to the atomized crystallizer, the atomized crystallizer is connected to the first storage tank, the atomized crystallizer and the bottom of the storage tank are respectively connected to the product area through pipelines, and connected to the upper part of the sub-distillation tower. The process includes opening the reboiler, evacuating the mother rectification tower and the sub-distillation tower, feeding the fraction to be separated into the mother rectification tower through the feed port, and extracting a large amount of dimethyl sulfone from the top of the sub-rectification tower. The top fraction of the sub-distillation tower is granulated and screened by an atomization crystallizer to obtain dimethyl sulfone product. In this process scheme, the mode of rectification and separation under vacuum state breaks the traditional long-term low-temperature crystallization and centrifugal separation mode, and greatly improves the purity and quality level of the product; the selected rectification equipment is double-tower rectification, which is shared by both towers Reboiler saves energy consumption.

Description

technical field [0001] The invention relates to a device and process for producing dimethyl sulfone by rectification with two towers, and belongs to the field of chemical equipment. Background technique [0002] In the production process of dimethyl sulfoxide, the intermediate product dimethyl sulfide is first synthesized, and the intermediate product dimethyl sulfide is further oxidized to obtain the target product dimethyl sulfoxide. Due to the specificity of the oxidation reaction and the need for safety control, the excess of the oxidant and the change of the residence time lead to a certain amount of dimethyl sulfoxide being further oxidized into dimethyl sulfone after oxidation. After rectification, the dimethyl sulfone in the still residue is extracted from the bottom of the dimethyl sulfoxide product tower, and then the crude dimethyl sulfone containing a certain amount of dimethyl sulfoxide and inorganic salts is recovered after crystallization and centrifugation. ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01D3/14B01D3/32C07C315/06C07C317/04
CPCB01D3/143B01D3/32B01D3/322C07C315/06C07C317/04
Inventor 王杰喻志勇杨军李修兵
Owner 新疆兴发化工有限公司
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