CN216837759U - Device for improving separation and concentration of dimethyl sulfoxide - Google Patents
Device for improving separation and concentration of dimethyl sulfoxide Download PDFInfo
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- CN216837759U CN216837759U CN202122933333.8U CN202122933333U CN216837759U CN 216837759 U CN216837759 U CN 216837759U CN 202122933333 U CN202122933333 U CN 202122933333U CN 216837759 U CN216837759 U CN 216837759U
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Abstract
The utility model discloses a device for improving dimethyl sulfoxide separation and concentration, wherein the bottom of a rectifying tower is connected with a finished product tower through a reboiler, the bottom of the finished product tower is connected with a residual kettle tank through the reboiler, the residual kettle tank is provided with a vacuum buffer tank, the vacuum buffer tank is connected with a first vacuum pump, and the residual kettle tank is connected to a crystallization kettle. The top of the rectifying tower is connected with a first condenser, the top of the first condenser is connected with a condensation storage tank, the bottom of the first condenser is connected with a water-containing sulfoxide groove, and the water-containing sulfoxide groove is connected with the upper part of the rectifying tower through a third vacuum pump. The utility model separates and concentrates dimethyl sulfoxide and dimethyl sulfone by azeotropic distillation and evaporation concentration; adopt this device can improve the output of dimethyl sulfoxide in the cauldron is incomplete, concentrated dimethyl sulfone does benefit to simultaneously and retrieves, increases the incomplete resource utilization of cauldron, improves the productivity effect.
Description
Technical Field
The utility model belongs to the field of production and preparation of dimethyl sulfoxide, and particularly relates to a device for improving sulfone separation and concentration.
Background
Dimethyl sulfoxide is colorless, viscous, transparent oily liquid or crystal. It is weakly alkaline, almost odorless, slightly bitter, and commonly used organic solvent. Dimethyl sulfoxide is widely used as a solvent and a reaction reagent, and is particularly used as a processing solvent and a spinning solvent in acrylonitrile polymerization, as a polyurethane synthesis and spinning solvent, as a synthesis solvent of polyamide, polyimide and polysulfone resin, as an aromatic hydrocarbon, a butadiene extraction solvent, a solvent for synthesizing chlorofluoroaniline and the like.
In the traditional sulphone salt concentration, a finished product tower is used for directly discharging kettle residues into a crystallization kettle for separation and concentration, the content of dimethyl sulfoxide in the kettle residues in the finished product tower is high, the dimethyl sulfone and the dimethyl sulfoxide are incompletely separated, and meanwhile, the kettle residues are directly fed into the crystallization kettle without being concentrated. In the process, the kettle residue is transferred in the kettle residue tank, and the dimethyl sulfoxide in the kettle residue can be completely separated in the finished product tower, so that the content of the dimethyl sulfoxide in the kettle residue is greatly reduced, the finished product extraction is increased, and the resource utilization rate is improved.
Disclosure of Invention
The utility model discloses a device and a process for improving dimethyl sulfoxide separation and concentration. Taking the residue (containing dimethyl sulfoxide and dimethyl sulfone) as a raw material, wherein the content ratio of the dimethyl sulfoxide to the dimethyl sulfone is 4-5: 2-3. Separating and concentrating dimethyl sulfoxide and dimethyl sulfone by azeotropic distillation and evaporation concentration. The process and the device can greatly improve the separation rate of the sulfone salt, improve the utilization rate of resources and increase the benefit of products. The process takes still residue (content ratio of dimethyl sulfone to radical sulfone) as a raw material, and comprises the following process steps:
separation and concentration: and controlling the temperature of the top of the tower by the finished product tower, and separating dimethyl sulfoxide from dimethyl sulfone in the kettle residue by distillation, wherein the gas phase of the finished product tower is dimethyl sulfoxide steam, and the liquid phase is dimethyl sulfone. Discharging the liquid phase to a kettle residue tank through an outlet valve, pumping the kettle residue into a crystallization kettle through a pump in the kettle residue tank, cooling and crystallizing, and extracting the finished product dimethyl sulfone.
The device used in the invention at least comprises the following equipment: finished product tower, rectifying column, reboiler, cauldron incomplete jar, crystallization kettle, and each equipment is connected as follows:
improve concentrated device of dimethyl sulfoxide separation, the rectifying column bottom is connected with the finished product tower through the reboiler, and the finished product tower bottom is connected with the incomplete jar of cauldron through the reboiler, is provided with the vacuum buffer tank on the incomplete jar of cauldron, is connected with vacuum pump one on the vacuum buffer tank, and the incomplete jar of cauldron is connected to crystallization kettle.
The top of the rectifying tower is connected with a first condenser, the top of the first condenser is connected with a condensation storage tank, the bottom of the first condenser is connected with a water-containing sulfoxide groove, and the water-containing sulfoxide groove is connected with the upper part of the rectifying tower through a third vacuum pump.
The finished product tower is connected with a second condenser, the top of the second condenser is connected with a condensation storage tank, the bottom of the second condenser is connected with a sulfoxide finished product tank, and the sulfoxide finished product tank is connected with the upper part of the finished product tower through a fourth vacuum pump. And a nitrogen inlet pipe is arranged on the residual kettle tank.
A process for improving the separation and concentration of dimethyl sulfoxide comprises the following steps:
the concentrated sulfoxide solution enters a rectifying tower, is heated by a reboiler for azeotropic rectification, and enters a finished product tower after being dehydrated;
controlling the temperature of the top of the finished product tower through a reboiler, vaporizing dimethyl sulfoxide in the material and extracting through a gas phase outlet at the top of the finished product tower, discharging kettle residual solution at the bottom of the finished product tower to a kettle residual tank through the reboiler, pumping the kettle residual solution in the kettle residual tank into a crystallization kettle, and extracting dimethyl sulfone from the crystallization kettle through cooling crystallization.
The concentrated sulfoxide solution has physical and chemical properties of dimethyl sulfoxide content of 75-80%, dimethyl sulfone content of 10-20% and water and salt content of 5-10%.
The temperature of the top of the rectifying tower is 45-55 ℃, gas phase materials at the top of the rectifying tower are condensed by a condenser, then the gas phase enters a condensation storage tank, liquid phase enters a water-containing sulfoxide groove and then enters the rectifying tower, wherein the physicochemical properties of the liquid phase comprise 75-85% of water and 15-25% of dimethyl sulfoxide.
The temperature of the top of the tower in the finished product tower is 119-123 ℃, gas-phase materials at the top of the tower are condensed by a condenser, then the gas phase enters a condensation storage tank, liquid phase enters a sulfoxide finished product tank, dimethyl sulfoxide with the mass concentration of more than 99.91% is obtained in the sulfoxide finished product tank, and the residual liquid enters the finished product tower.
And (3) after the pressure in the residual kettle tank is pumped to-100 to-50 KPa, discharging the residual kettle liquid from the finished product tower to the residual kettle tank, closing the vacuum when the liquid level in the residual kettle tank is 90% or more, starting to fill nitrogen into the residual kettle tank, pressing the residual kettle to a crystallization kettle through the nitrogen, pressing the residual kettle tank to the crystallization kettle through the nitrogen, cooling and crystallizing, and extracting the finished product dimethyl sulfone.
Vacuum is needed in the residual kettle tank firstly, and then residual liquid is discharged, because the rectification finished product system is a vacuum system, the pressure is about-60 kpa, if the residual kettle tank breaks the vacuum of the rectification finished product system under normal pressure, production is influenced, and materials cannot be discharged into the residual kettle tank.
The purpose of filling nitrogen is to pressurize the kettle residue tank so as to press the materials from the first floor kettle residue tank into the third floor crystallization kettle (the crystallization kettle is a normal pressure device). The purity of the product is improved.
The temperature of the top of the finished product tower needs to be controlled at the boiling point temperature of the dimethyl sulfoxide under the residual pressure, otherwise, the separation is incomplete. When the finished product tower discharges kettle residues, the kettle residue tank needs to be vacuumized.
Drawings
FIG. 1 is a schematic diagram of an apparatus for enhancing separation and concentration of dimethyl sulfoxide.
1. The system comprises a rectifying tower, 2 parts of a reboiler, 3 parts of a finished product tower, 4 parts of a kettle residue tank, 5 parts of a vacuum buffer tank, 6 parts of a first condenser, 7 parts of a second condenser, 8 parts of a condensation storage tank, 9 parts of a sulfoxide finished product tank, 10 parts of a water-containing sulfoxide tank, 11 parts of a nitrogen inlet pipe, a part of a first vacuum pump, b parts of a second vacuum pump, c parts of a third vacuum pump and d parts of a fourth vacuum pump.
Detailed Description
The utility model is further described with reference to the following figures and examples, but the scope of the patent claims is not limited to the examples.
Example 1
The utility model provides an improve concentrated device of dimethyl sulfoxide separation, 1 bottom of rectifying column is connected with finished product tower 3 through reboiler 2, and 3 bottoms of finished product tower are connected with the incomplete jar 4 of cauldron through reboiler 2, are provided with vacuum buffer tank 5 on the incomplete jar 4 of cauldron, are connected with a vacuum pump a on the vacuum buffer tank 5, and the incomplete jar 4 of cauldron is connected to crystallization kettle. The top of the rectifying tower 1 is connected with a first condenser 6, the top of the first condenser 6 is connected with a condensation storage tank 8, the bottom of the first condenser 6 is connected with a water-containing sulfoxide groove 10, and the water-containing sulfoxide groove 10 is connected with the upper part of the rectifying tower 1 through a third vacuum pump c. The finished product tower 3 is connected with a second condenser 7, the top of the second condenser 7 is connected with a condensation storage tank 8, the bottom of the second condenser 7 is connected with a sulfoxide finished product tank 9, and the sulfoxide finished product tank 9 is connected with the upper part of the finished product tower 3 through a fourth vacuum pump d. The residual kettle tank 4 is provided with a nitrogen inlet pipe 11.
Example 2
A process for improving the separation and concentration of dimethyl sulfoxide comprises the following steps:
the concentrated sulfoxide solution has physical and chemical properties of dimethyl sulfoxide content of 84-89%, dimethyl sulfone content of 10-15% and water content and salt content of 1-2%.
The concentrated sulfoxide solution enters a rectifying tower, is heated to 155-158 ℃ by a reboiler for azeotropic rectification, and enters a finished product tower after being dehydrated; gas phase materials at the top of the tower are condensed by a condenser I6, then the gas phase enters a condensation storage tank 8, liquid phase enters a water-containing sulfoxide groove 10 and then enters a rectifying tower 1, wherein the physicochemical properties of the liquid phase are that the water content is 1-2 percent, and the dimethyl sulfoxide content is 98-99.5 percent.
Controlling the temperature at the top of the finished product tower to 119-123 ℃ by a reboiler, and separating dimethyl sulfoxide from dimethyl sulfone in kettle residues (the kettle residues contain 70% of dimethyl sulfoxide and 30% of dimethyl sulfone) by evaporation concentration, wherein the gas phase of the finished product tower is dimethyl sulfoxide vapor, and the liquid phase is dimethyl sulfone. The gas phase material at the top of the tower is condensed by a condenser I6, the gas phase enters a condensation storage tank 8, the liquid phase enters a sulfoxide finished product tank 9, dimethyl sulfoxide with the mass concentration of 99.97% is obtained in the sulfoxide finished product tank 9, the water content is 200PPM, the yield is 90.6%, the residual liquid enters a finished product tower 3, and the purity of the dimethyl sulfoxide is 70.5%.
After the pressure in the residual kettle tank 4 is pumped to-50 KPa, discharging kettle residual liquid from the product tower 3 to the residual kettle tank 4, when the liquid level in the residual kettle tank 4 is 99%, closing the vacuum, starting to charge nitrogen into the residual kettle tank 4, pressing the kettle residual liquid to a crystallization kettle through the nitrogen, pressing the kettle residual liquid to the crystallization kettle through the nitrogen pressure in the residual kettle tank to the crystallization kettle, cooling and crystallizing to extract a finished product of dimethyl sulfone, wherein the purity of the dimethyl sulfone is 96.5%.
Claims (4)
1. The utility model provides an improve concentrated device of dimethyl sulfoxide separation, its characterized in that, rectifying column (1) bottom is connected with finished product tower (3) through reboiler (2), and finished product tower (3) bottom is connected with incomplete jar of cauldron (4) through reboiler (2), is provided with vacuum buffer tank (5) on the incomplete jar of cauldron (4), is connected with vacuum pump (a) on vacuum buffer tank (5), and the incomplete jar of cauldron (4) are connected to the crystallization kettle.
2. The device for improving the separation and concentration of dimethyl sulfoxide according to claim 1, wherein the top of the rectifying tower (1) is connected with a first condenser (6), the top of the first condenser (6) is connected with a condensation storage tank (8), the bottom of the first condenser (6) is connected with a water-containing sulfoxide tank (10), and the water-containing sulfoxide tank (10) is connected with the upper part of the rectifying tower (1) through a third vacuum pump (c).
3. The device for improving the separation and concentration of dimethyl sulfoxide according to claim 1, wherein the finished product tower (3) is connected with a second condenser (7), the top condensation storage tank (8) of the second condenser (7) is connected, the bottom of the second condenser (7) is connected with a sulfoxide finished product tank (9), and the sulfoxide finished product tank (9) is connected with the upper part of the finished product tower (3) through a fourth vacuum pump (d).
4. The device for improving the separation and concentration of dimethyl sulfoxide according to claim 1, wherein a nitrogen inlet pipe (11) is arranged on the still residue tank (4).
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122933333.8U CN216837759U (en) | 2021-11-26 | 2021-11-26 | Device for improving separation and concentration of dimethyl sulfoxide |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122933333.8U CN216837759U (en) | 2021-11-26 | 2021-11-26 | Device for improving separation and concentration of dimethyl sulfoxide |
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| CN216837759U true CN216837759U (en) | 2022-06-28 |
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| CN202122933333.8U Active CN216837759U (en) | 2021-11-26 | 2021-11-26 | Device for improving separation and concentration of dimethyl sulfoxide |
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2021
- 2021-11-26 CN CN202122933333.8U patent/CN216837759U/en active Active
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