CN212560057U - Molecular sieve dehydration system for dimethyl sulfoxide - Google Patents
Molecular sieve dehydration system for dimethyl sulfoxide Download PDFInfo
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- CN212560057U CN212560057U CN202020209668.8U CN202020209668U CN212560057U CN 212560057 U CN212560057 U CN 212560057U CN 202020209668 U CN202020209668 U CN 202020209668U CN 212560057 U CN212560057 U CN 212560057U
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Abstract
The molecular sieve dehydration system for dimethyl sulfoxide comprises a rectifying tower (1), a first molecular sieve dehydration tower (2), a second molecular sieve dehydration tower (2'), a gas-liquid phase separation tank (3) and a nitrogen source; the rectifying tower is used for rectifying the aqueous dimethyl sulfoxide solution to separate part of water; the two molecular sieve dehydration towers are both connected with the rectifying tower and are used for adsorbing the water-containing dimethyl sulfoxide from which part of water is separated so as to further dehydrate; a nitrogen source is connected to the two molecular sieve dehydration towers and is used for replacing and discharging residual aqueous dimethyl sulfoxide solution in the towers; the gas-liquid phase separation tank is respectively connected with the two molecular sieve dehydration towers so as to carry out gas-liquid separation on the replaced or regenerated substances in the molecular sieve dehydration towers, and the separated nitrogen is sent into the molecular sieve dehydration towers for cyclic utilization; the gas-liquid phase separation tank is connected with the rectifying tower and is used for sending the separated liquid phase to the rectifying tower for reprocessing.
Description
Technical Field
The utility model relates to a solvent recovery technical field, concretely relates to a molecular sieve dewatering system for dimethyl sulfoxide and dehydration method thereof.
Background
Dimethyl sulfoxide (DMSO) is a sulfur-containing organic compound, is colorless and odorless transparent liquid at normal temperature, is liquid with strong hygroscopicity, has the characteristics of high polarity, high boiling point, good thermal stability, non-proton and water miscibility, can be dissolved in most organic matters such as ethanol, propanol, benzene, chloroform and the like, and is known as an 'universal solvent'. It can be used as organic solvent, reaction medium and intermediate for organic synthesis, and also as absorbent for recovering acetylene and sulfur dioxide. Because dimethyl sulfoxide has strong hygroscopicity, dimethyl sulfoxide is easy to absorb moisture when used as a solvent or an absorbent, so that the concentration is reduced, and the dehydration link of dimethyl sulfoxide is a technical problem which needs to be solved in order to realize recycling.
SUMMERY OF THE UTILITY MODEL
The utility model aims to solve the recovery and cyclic utilization problem of water-containing dimethyl sulfoxide, provide a molecular sieve dewatering system and dehydration method for dimethyl sulfoxide, this system utilizes two molecular sieve dehydration towers to carry out alternate use (a molecular sieve dehydration tower gets into the molecular sieve regeneration step after using the saturation and handles, the molecular sieve dehydration tower that takes over begins to work, guarantee that the dehydration process is incessant), perhaps use simultaneously according to the ageing requirement, the dimethyl sulfoxide that the system of the invention can realize after the dehydration is more than or equal to 99.9% according to the mass percentage.
The invention has the technical scheme that the molecular sieve dehydration system for the dimethyl sulfoxide comprises a rectifying tower, a first molecular sieve dehydration tower, a second molecular sieve dehydration tower, a gas-liquid phase separation tank and a nitrogen source; the rectifying tower is used for rectifying the aqueous dimethyl sulfoxide solution so as to separate part of water in the aqueous dimethyl sulfoxide solution; the first molecular sieve dehydration tower is connected to the rectifying tower through a first valve; the second molecular sieve dehydration tower is connected to the rectifying tower through a second valve, so that the aqueous dimethyl sulfoxide solution from which part of water is separated is adsorbed in one molecular sieve dehydration tower or two molecular sieve dehydration towers simultaneously, and further dehydration is realized; the nitrogen source is respectively connected with the first molecular sieve dehydration tower and the second molecular sieve dehydration tower and is used for feeding nitrogen into the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower so as to replace residual aqueous dimethyl sulfoxide solution in the molecular sieve dehydration tower and discharge the residual aqueous dimethyl sulfoxide solution out of the molecular sieve dehydration tower through the nitrogen; the gas-liquid phase separation tank is connected with the first molecular sieve dehydration tower through a first pipeline, a third valve arranged on the first pipeline, a second pipeline and a fourth valve arranged on the second pipeline; the gas-liquid phase separation tank is also connected with the second molecular sieve dehydration tower through a third pipeline, a fifth valve arranged on the third pipeline, a fourth pipeline and a sixth valve arranged on the fourth pipeline, so that nitrogen in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower and aqueous dimethyl sulfoxide solution displaced by the nitrogen and discharged are sent into the gas-liquid phase separation tank through the first pipeline and/or the third pipeline for gas-liquid separation treatment, and then the nitrogen separated by the gas-liquid phase separation tank is sent into the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower through the second pipeline and/or the fourth pipeline for cyclic utilization; the bottom of the gas-liquid phase separation tank is connected with a liquid phase pipeline inlet of the rectifying tower and is used for sending the water-containing dimethyl sulfoxide solution separated from the gas-liquid phase separation tank to the rectifying tower for reprocessing.
The rectifying tower is one of the important parts for removing most of water from the aqueous dimethyl sulfoxide solution, and the water is removed in the boiling rectifying process, so that the adsorption requirement of the molecular sieve in the subsequent molecular sieve dehydrating tower can be reduced, and the replacement frequency of the molecular sieve can be greatly reduced.
The invention designs a bimolecular sieve dehydration tower which is respectively connected with a rectifying tower through respective valves, when in use, one molecular sieve dehydration tower is preferably adopted to adsorb firstly, the other molecular sieve dehydration tower is used to adsorb after the adsorption is saturated, and the adsorbed liquid phase enters the step of molecular sieve regeneration treatment, so as to displace and discharge the adsorbed liquid phase, to replace the molecular sieve dehydration tower in use in time; when the flow rate of the tower bottom material of the rectifying tower to be treated is large or the time requirement is urgent, two molecular sieve dehydration towers can be used simultaneously, so that the tower bottom material of the rectifying tower flows into the two molecular sieve dehydration towers simultaneously to be adsorbed respectively.
The nitrogen source and the gas-liquid phase separation tank are respectively connected with the two molecular sieve dehydration towers, which is equivalent to the mirror image replication with one molecular sieve dehydration tower, and the connection mode and the function are basically consistent in the two molecular sieve dehydration towers.
Further, the molecular sieve dehydration system for dimethyl sulfoxide of the invention further comprises a reboiler, a condensation heat exchanger, a second condensation heat exchanger, a heater, a second heater, a seventh valve, an eighth valve, a moisture detector and a second moisture detector; the reboiler is connected to the bottom of the rectifying tower and is used for boiling and rectifying the aqueous dimethyl sulfoxide solution in the rectifying tower; the first molecular sieve dehydration tower and the second molecular sieve dehydration tower are respectively connected with a condensation heat exchanger and a second condensation heat exchanger and are used for transferring heat generated in the molecular sieve adsorption process in the molecular sieve dehydration tower; a connecting pipeline between the nitrogen source and the first molecular sieve dehydration tower and a second pipeline between the gas-liquid phase separation tank and the first molecular sieve dehydration tower are combined into a first nitrogen pipeline, and the heater and a seventh valve are arranged on the first nitrogen pipeline in parallel; a connecting pipeline between the nitrogen source and the second molecular sieve dehydration tower and a fourth pipeline between the gas-liquid phase separation tank and the second molecular sieve dehydration tower are combined into a second nitrogen pipeline, and the second heater and the eighth valve are arranged on the second nitrogen pipeline in parallel; the heater and the second heater are heated by steam or electricity and used for heating the nitrogen flowing through and then sending the nitrogen into the molecular sieve dehydration tower, and the seventh valve and the eighth valve are used for adjusting and controlling the unheated nitrogen flowing through to enter the molecular sieve dehydration tower so as to finally adjust the temperature of the nitrogen entering the molecular sieve dehydration tower; and the moisture detector and the second moisture detector are respectively connected with the tops of the first molecular sieve dehydration tower and the second molecular sieve dehydration tower and are used for detecting the water content in the dimethyl sulfoxide discharged from the tops of the molecular sieve dehydration towers.
The system mainly comprises a rectifying tower, wherein most of water in the water-containing dimethyl sulfoxide solution is separated and removed by a rectifying means, the water content in the water-containing dimethyl sulfoxide solution is lowered to a lower level, and then the water-containing dimethyl sulfoxide solution enters a molecular sieve dehydration tower, and most of water is removed by utilizing the water absorption and dehydration properties of a molecular sieve, so that the dimethyl sulfoxide solvent with higher purity is obtained.
When the water absorption capacity of the molecular sieve in the molecular sieve dehydration tower reaches saturation, according to the service conditions of two molecular sieve dehydration towers, when using one of the molecular sieve dehydration towers, closing the communication between the molecular sieve dehydration tower and the rectifying tower, opening the communication between the other molecular sieve dehydration tower and the rectifying tower, ensuring that the adsorption is continuously carried out, and simultaneously utilizing hot nitrogen to carry out gas replacement and molecular sieve regeneration in the tower on the molecular sieve dehydration tower disconnected from the communication: displacing most of the accumulated water-containing dimethyl sulfoxide solution into a gas-liquid phase-splitting tank through nitrogen with pressure, recycling gas-phase nitrogen, returning the water-containing dimethyl sulfoxide solution at the bottom of the tank to a rectifying tower, regenerating a molecular sieve in a molecular sieve dehydration tower under negative pressure after displacement is finished, removing and separating water in pore channels of the molecular sieve and the water-containing dimethyl sulfoxide solution, transferring the water-containing dimethyl sulfoxide solution to the gas-liquid phase-splitting tank, and then returning the water-containing dimethyl sulfoxide solution to the rectifying tower through a pipeline at the bottom of the tank; the molecular sieve dehydration column which completes the above-mentioned gas replacement in the column and molecular sieve regeneration is used as a continuous substitute for the molecular sieve dehydration column being adsorbed.
In another aspect, the present invention provides a molecular sieve dehydration method for dimethyl sulfoxide, which utilizes the molecular sieve dehydration system for dimethyl sulfoxide, and the dehydration process comprises the following steps:
s1, feeding the water-containing dimethyl sulfoxide solution into a rectifying tower, and separating part of water in the water-containing dimethyl sulfoxide solution through a rectifying process, wherein the separated water is extracted from the top of the rectifying tower, and the water-containing dimethyl sulfoxide solution from which part of water is separated is arranged at the bottom of the rectifying tower;
and S2, feeding the bottom material of the rectifying tower from the bottom of the first molecular sieve dehydrating tower and/or the bottom of the second molecular sieve dehydrating tower, dehydrating through the adsorption action of the molecular sieve filled in the molecular sieve dehydrating tower, and extracting the dehydrated dimethyl sulfoxide from the top of the molecular sieve dehydrating tower to be recycled.
Further, when the water content in the dimethyl sulfoxide extracted from the top of the first molecular sieve dehydrating tower and/or the second molecular sieve dehydrating tower in the step S2 is more than 0.1% by weight, closing a valve between the molecular sieve dehydrating tower and the rectifying tower, disconnecting the molecular sieve dehydrating tower communicated with the rectifying tower, and allowing the molecular sieve dehydrating tower to enter a molecular sieve regenerating step: the molecular sieve regeneration step specifically comprises a step S3 of replacing residual water-containing dimethyl sulfoxide in a molecular sieve dehydration tower by nitrogen, and a step S4 of dehydrating by a negative pressure molecular sieve; the step S3 is: one path of nitrogen of the nitrogen source is heated by a heater and/or a second heater and then is sent into the molecular sieve dehydration tower from the bottom of the molecular sieve dehydration tower, and meanwhile, the other path of unheated nitrogen flows through a seventh valve and/or an eighth valve and is sent into the molecular sieve dehydration tower from the bottom of the molecular sieve dehydration tower after being regulated, so that the temperature of the nitrogen entering the molecular sieve dehydration tower is controlled; replacing free water-containing dimethyl sulfoxide solution in the molecular sieve dehydration tower by nitrogen, and discharging the water-containing dimethyl sulfoxide solution replaced by the nitrogen and the nitrogen into a gas-liquid phase-splitting tank until the water-containing dimethyl sulfoxide solution in the molecular sieve dehydration tower is completely replaced; the nitrogen and the water-containing dimethyl sulfoxide solution entering the gas-liquid phase separation tank are subjected to gas-liquid separation, and the gas-phase nitrogen serving as a part of the nitrogen source in the step S3 enters the molecular sieve dehydration tower to be recycled; returning the water-containing dimethyl sulfoxide solution to the rectifying tower for secondary water separation, and then entering the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower for dehydration; the step S4 is: forming a negative pressure environment in the molecular sieve dehydration tower so as to dehydrate and regenerate the molecular sieve in the molecular sieve dehydration tower, sending the nitrogen and the removed liquid phase into a gas-liquid phase separation tank for condensation and separation, and finally obtaining and separating a gas phase which is the nitrogen and used as a part of the nitrogen source in the step S3 to enter the molecular sieve dehydration tower for cyclic utilization; the liquid phase is sent to a rectifying tower to carry out the dehydration treatment process again.
Wherein, it is determined industrially according to the liquid content in the gas, and the dimethyl sulfoxide solution is considered to be completely replaced as long as the replacement gas entering the gas-liquid phase separation tank has no liquid phase; in the actual process, a small amount of dimethyl sulfoxide enters the molecular sieve during the adsorption dehydration process of the molecular sieve in step S2, including free dimethyl sulfoxide in the molecular sieve dehydration tower, and is not replaced by 100% in the nitrogen replacement step of step S3, so that all regenerated gas phases in the molecular sieve dehydration tower under the negative pressure in step S4 contain nitrogen, water and aqueous dimethyl sulfoxide solution, and the gas phases contain not only nitrogen, but also water and aqueous dimethyl sulfoxide solution, and need to enter the gas-liquid phase separation tank for condensation and separation, the nitrogen is still a gas phase, and the separated liquid phase contains water and aqueous dimethyl sulfoxide solution, so that the liquid phase formed by condensation after entering the gas-liquid phase separation tank in step S4 needs to be returned to the rectification tower for re-dehydration treatment to recover dimethyl sulfoxide therein.
Furthermore, the pressure in the rectifying tower in the S1 is (-0.01) (-0.08) MPa, the temperature of the bottom of the rectifying tower controlled by a reboiler is 90-130 ℃, and the temperature of the top of the rectifying tower is 50-80 ℃.
Further, in the step S2, the temperature in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower is controlled within a range of 20 to 60 ℃ by heat exchange of the condensation heat exchanger or the second condensation heat exchanger.
Furthermore, in the step S2, the molecular sieve filled in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower is one of 3A, 4A and 5A molecular sieves, and the particle size of the molecular sieve is 1 to 6 mm.
Furthermore, in step S3, the temperature of the nitrogen gas entering the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower is controlled to be 30 to 80 ℃, and the pressure in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower is controlled to be 0.1 to 0.3 MPa.
Furthermore, the negative pressure environment in step S4 means that the pressure in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower is (-0.01) — (-0.08) MPa, and the temperature in the first molecular sieve dehydration tower and/or the second molecular sieve dehydration tower in the molecular sieve regeneration stage in step S4 is 60 to 100 ℃.
Further, the water content of the dimethyl sulfoxide extracted from the top of the first molecular sieve dehydrating tower and/or the second molecular sieve dehydrating tower in the step S2 is less than or equal to 0.1% by mass.
Further, the water content of the dimethyl sulfoxide collected from the top of the molecular sieve dehydration tower in the step S2 is not more than 0.1% by mass.
The molecular sieve dehydration system for dimethyl sulfoxide and the dehydration process thereof can realize continuous removal of water in water-containing dimethyl sulfoxide solution and timely regeneration treatment of the molecular sieve, realize recycling of dimethyl sulfoxide, and have the advantages of simple equipment, cyclic utilization of resources, continuous process and no generation of industrial harmful substances.
Drawings
These and/or other aspects and advantages of the present invention will become more apparent and more readily appreciated from the following detailed description of the embodiments of the invention, taken in conjunction with the accompanying drawings of which:
FIG. 1 is a schematic diagram of a molecular sieve dehydration system for dimethyl sulfoxide and a process for dehydrating an aqueous dimethyl sulfoxide solution, according to an embodiment of the invention:
wherein 1-a rectifying tower, 2-a first molecular sieve dehydrating tower and 2' -a second molecular sieve dehydrating tower; 3-a gas-liquid phase separation tank, 4-a reboiler, 5-a condensing heat exchanger, 5 ' -a second condensing heat exchanger, 6-a heater, 6 ' -a second heater, 8-a moisture detector, 8 ' -a second moisture detector, 7-a seventh valve, 7 ' -an eighth valve, 9-a third valve and 9 ' -a fifth valve; 10-fourth valve, 10' -sixth valve.
Detailed Description
In order that those skilled in the art will better understand the present invention, the following detailed description of the invention is provided in conjunction with the accompanying drawings and the detailed description of the invention.
Example 1
A molecular sieve dehydration system for dimethyl sulfoxide is shown in figure 1 and comprises a rectifying tower 1, a first molecular sieve dehydration tower 2, a second molecular sieve dehydration tower 2 ', a gas-liquid phase separation tank 3, a reboiler 4, a condensing heat exchanger 5, a second condenser 5', a heater 6, a second heater 6 ', a moisture detector 8, a second moisture detector 8', a nitrogen source and a plurality of valves; the rectifying tower 1 is used for rectifying the aqueous dimethyl sulfoxide solution to separate part of water in the aqueous dimethyl sulfoxide solution; the first molecular sieve dehydration tower 2 is connected with the rectifying tower 1 through a first valve 11 and is used for separating partial water of the water-containing dimethyl sulfoxide in the rectifying tower 1 to enter the water-containing dimethyl sulfoxide to be adsorbed by a molecular sieve so as to realize further dehydration; the nitrogen source is connected with the first molecular sieve dehydration tower 2 through a heater 6 and is used for feeding nitrogen into the molecular sieve dehydration tower 2 so as to replace and discharge residual aqueous dimethyl sulfoxide solution in the tower; the gas-liquid phase separation tank 3 is respectively connected with the first molecular sieve dehydration tower 2 through a first pipeline and a third valve 9 arranged on the first pipeline, and a second pipeline and a fourth valve 10 arranged on the second pipeline, so that substances in the first molecular sieve dehydration tower 2 are sent into the gas-liquid phase separation tank 3 through the first pipeline for gas-liquid separation treatment, and then the separated nitrogen is sent into the first molecular sieve dehydration tower 2 through the second pipeline for recycling; the rectification column 1, nitrogen gas source, and vapor-liquid phase separation tank 3 are also connected to the second molecular sieve dehydration column 2' in the same manner and for the same purpose as the connection of the first molecular sieve dehydration column 2 described above, specifically: the second molecular sieve dehydration tower 2 'is connected with the rectifying tower 1 through a second valve 11' and is used for separating partial water of the water-containing dimethyl sulfoxide in the rectifying tower 1 to enter the water-containing dimethyl sulfoxide to be adsorbed by a molecular sieve so as to realize further dehydration; the nitrogen source is connected with the second molecular sieve dehydration tower 2 'through a second heater 6' and is used for feeding nitrogen into the second molecular sieve dehydration tower to replace and discharge residual aqueous dimethyl sulfoxide solution in the tower; the gas-liquid phase separation tank 3 is respectively connected with the second molecular sieve dehydration tower 2 ' through a third pipeline and a fifth valve 9 ' arranged on the third pipeline, and a fourth pipeline and a sixth valve 10 ' arranged on the fourth pipeline, so that substances in the second molecular sieve dehydration tower 2 ' are sent into the gas-liquid phase separation tank 3 through the third pipeline for gas-liquid separation treatment, and then the separated nitrogen is sent into the second molecular sieve dehydration tower 2 ' through the fourth pipeline for recycling;
the bottom of the gas-liquid phase separation tank 3 is connected with the rectifying tower 1 and is used for sending the aqueous dimethyl sulfoxide solution separated from the gas-liquid phase separation tank 3 to the rectifying tower 1 for reprocessing; the reboiler 4 is connected with the rectifying tower 1 and is used for boiling and rectifying the water-containing dimethyl sulfoxide solution in the rectifying tower 1; the condensation heat exchanger 5 and the condensation heat exchanger 5 'are respectively connected with the first molecular sieve dehydration tower 2 and the second molecular sieve dehydration tower 2' and are used for transferring heat generated in the process that the water-containing dimethyl sulfoxide solution is adsorbed by the molecular sieve in the molecular sieve dehydration tower; preferably, the connecting pipeline between the nitrogen source and the first molecular sieve dehydration tower 2 and the second pipeline between the gas-liquid phase separation tank 3 and the first molecular sieve dehydration tower 2 are merged into a first nitrogen pipeline, the heater 6 is arranged on the first nitrogen pipeline and connected with a seventh valve 7 in parallel, and similarly, the connecting pipeline between the nitrogen source and the second molecular sieve dehydration tower 2 'and the fourth pipeline between the gas-liquid phase separation tank 3 and the second molecular sieve dehydration tower 2' are merged into a second nitrogen pipeline, the second heater 6 'is arranged on the second nitrogen pipeline and connected with an eighth valve 7' in parallel, the heater 6 and the second heater 6 'are used for steam heating or electric heating and are used for heating the nitrogen flowing through and then feeding the nitrogen into the respectively connected molecular sieve dehydration towers, and the seventh valve 7' are used for regulating and controlling the non-heated nitrogen flowing through to enter the respectively connected molecular sieve dehydration towers, to finally regulate the temperature of the nitrogen entering the molecular sieve dehydration tower; the moisture detector 8 and the second moisture detector 8 'are respectively connected to the tops of the first molecular sieve dehydration tower 2 and the second molecular sieve dehydration tower 2', and are used for detecting the water content in the dimethyl sulfoxide discharged from the tops of the respectively connected molecular sieve dehydration towers.
Example 2
A molecular sieve dehydration method of dimethyl sulfoxide using the molecular sieve dehydration system for dimethyl sulfoxide of example 1, the dehydration process comprising the steps of:
s1, feeding the water-containing dimethyl sulfoxide solution into a rectifying tower 1, and separating part of water in the water-containing dimethyl sulfoxide solution through a rectifying process, wherein the separated water is extracted from the top of the rectifying tower 1, and the water-containing dimethyl sulfoxide solution from which part of water is separated is arranged at the bottom of the rectifying tower 1; wherein the pressure in the rectifying tower 1 is-0.01 to-0.08 MPa, the tower kettle temperature of the rectifying tower 1 controlled by the reboiler 4 is 90 to 130 ℃, and the tower top temperature is 50 to 80 ℃;
s2, opening the first valve 11 (keeping the second valve 11' closed), sending the water-containing dimethyl sulfoxide solution with part of water separated out into the first molecular sieve dehydration tower from the bottom of the first molecular sieve dehydration tower through the first valve 11, dehydrating through the adsorption action of the molecular sieve filled in the first molecular sieve dehydration tower 2, and extracting the dehydrated dimethyl sulfoxide from the top of the first molecular sieve dehydration tower 2 for recycling; wherein the temperature in the molecular sieve dehydration tower 2 is controlled within the range of 20-60 ℃ through heat exchange of a condensation heat exchanger 5; the filled molecular sieve is one of 3A, 4A and 5A molecular sieves, and the particle size of the molecular sieve is 1-6 mm; observing the water content of the dimethyl sulfoxide extracted from the tower top, and keeping the water content of the dimethyl sulfoxide to be less than or equal to 0.1 percent by mass;
s3, when the water content of dimethyl sulfoxide extracted from the top of the first molecular sieve dehydration tower 2 is more than 0.1% by mass percent, closing the first valve 11, opening the second valve 11 ', so that the bottom material of the rectification tower is sent into the second molecular sieve dehydration tower from the bottom of the second molecular sieve dehydration tower through the second valve 11', the dehydration is carried out through the adsorption action of the molecular sieve filled in the second molecular sieve dehydration tower 2 ', and the dehydrated dimethyl sulfoxide is extracted from the top of the second molecular sieve dehydration tower 2' and is recycled;
s4, performing a molecular sieve regeneration process on the first molecular sieve dehydration tower 2 while performing step S3, specifically including a step S41 of replacing residual aqueous dimethyl sulfoxide in the molecular sieve dehydration tower 2 with nitrogen, and a step S42 of dehydrating with a negative pressure molecular sieve:
s41, heating one path of nitrogen of a nitrogen source by a heater 6, sending the heated nitrogen into a first molecular sieve dehydration tower 2 from the bottom of the first molecular sieve dehydration tower 2, adjusting the flow of the unheated nitrogen by a seventh valve 7, and sending the heated nitrogen into the first molecular sieve dehydration tower 2 from the bottom of the first molecular sieve dehydration tower 2, so as to control the temperature of the nitrogen entering the first molecular sieve dehydration tower 2, wherein the temperature of the nitrogen entering the first molecular sieve dehydration tower 2 is controlled to be 30-80 ℃, and the pressure in the first molecular sieve dehydration tower 2 is 0.1-0.3 MPa; replacing the free water-containing dimethyl sulfoxide solution in the first molecular sieve dehydration tower 2 by nitrogen, and discharging the nitrogen and the replaced water-containing dimethyl sulfoxide solution into a gas-liquid phase-splitting tank 3 until the free water-containing dimethyl sulfoxide solution in the first molecular sieve dehydration tower 2 is completely replaced; the nitrogen and the water-containing dimethyl sulfoxide solution entering the gas-liquid phase separation tank 3 are subjected to gas-liquid separation, and the gas-phase nitrogen serving as a part of the nitrogen source in the step S3 enters the first molecular sieve dehydration tower 2 through a second pipeline or a first nitrogen pipeline to be recycled; returning the water-containing dimethyl sulfoxide solution to the rectifying tower 1 for water separation again, and then entering a first molecular sieve dehydration tower 2 for dehydration;
s42, forming a negative pressure environment (the pressure is-0.08 MPa) in the first molecular sieve dehydration tower 2, and controlling the temperature to be 60-100 ℃ so as to dehydrate and regenerate the molecular sieve in the first molecular sieve dehydration tower 2, sending the nitrogen and the removed gas phase into the gas-liquid phase separation tank 3 for condensation and separation, wherein the finally obtained and separated gas phase is nitrogen, and the nitrogen is used as a part of the nitrogen source in the step S3 and enters the molecular sieve dehydration tower 2 through a second pipeline or a first nitrogen pipeline for recycling; part of the gas phase is condensed into a liquid phase and sent to the rectifying tower 1 for carrying out the dehydration treatment again.
Example 3
Alternative and alternative processing operations for example 2, those skilled in the art are familiar with the following conventional operations in the art:
1) the step S4 in the above embodiment 2 may further include continuously replacing the second molecular sieve dehydrating tower 2' that has been saturated by adsorption with the first molecular sieve dehydrating tower 2 after the molecular sieve regeneration treatment, and cyclically replacing the two towers to ensure that the dehydration treatment process is uninterrupted until all the solution to be treated is completed;
2) when the second valve 11 is opened and the first valve 11 is closed in step S2 of the above embodiment 2, the second molecular sieve dehydration column 2 'is used for dehydration in step S2, and the second molecular sieve dehydration column 2' saturated by adsorption is replaced with the first molecular sieve dehydration column 2 in step S3; step S4, carrying out molecular sieve regeneration treatment on the second molecular sieve dehydration tower 2' which is saturated by adsorption;
3) when the second valve 11 and the first valve 11 are opened simultaneously in step S2 in the above example 2, and the two molecular sieve dehydration columns are operated synchronously, the water content of dimethyl sulfoxide in the top of which molecular sieve dehydration column in step S3 is greater than 0.1% by mass, the valve between the molecular sieve dehydration column and the rectification column 1 is first closed, and the molecular sieve regeneration treatment in step S4 is performed on the column.
While various embodiments of the present invention have been described above, the above description is intended to be illustrative, not exhaustive, and not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. Therefore, the protection scope of the present invention shall be subject to the protection scope of the claims.
Claims (2)
1. A molecular sieve dehydration system for dimethyl sulfoxide is characterized by comprising a rectifying tower (1), a first molecular sieve dehydration tower (2) and a second molecular sieve dehydration tower (2'), a gas-liquid phase separation tank (3) and a nitrogen source;
the rectifying tower (1) is used for rectifying the aqueous dimethyl sulfoxide solution to separate part of water in the aqueous dimethyl sulfoxide solution;
the first molecular sieve dehydration tower (2) is connected to the rectifying tower (1) through a first valve (11); the second molecular sieve dehydration tower (2 ') is connected to the rectification tower (1) through a second valve (11') so that the aqueous dimethyl sulfoxide solution from which part of water is separated is adsorbed in one molecular sieve dehydration tower or two molecular sieve dehydration towers at the same time to realize further dehydration;
the nitrogen source is respectively connected with the first molecular sieve dehydration tower (2) and the second molecular sieve dehydration tower (2 ') and is used for feeding nitrogen into the first molecular sieve dehydration tower (2) and/or the second molecular sieve dehydration tower (2') so as to replace residual aqueous dimethyl sulfoxide solution in the molecular sieve dehydration towers by the nitrogen and discharge the residual aqueous dimethyl sulfoxide solution out of the molecular sieve dehydration towers;
the gas-liquid phase separation tank (3) is connected with the first molecular sieve dehydration tower (2) through a first pipeline and a third valve (9) arranged on the first pipeline, and a second pipeline and a fourth valve (10) arranged on the second pipeline; the gas-liquid phase separation tank (3) is also connected with the second molecular sieve dehydration tower (2 ') through a third pipeline and a fifth valve (9 ') arranged on the third pipeline, a fourth pipeline and a sixth valve (10 ') arranged on the fourth pipeline, so that nitrogen in the first molecular sieve dehydration tower (2) and/or the second molecular sieve dehydration tower (2 ') and aqueous dimethyl sulfoxide solution displaced by the nitrogen and discharged are sent into the gas-liquid phase separation tank (3) through the first pipeline and/or the third pipeline for gas-liquid separation treatment, and then the nitrogen separated from the gas-liquid phase separation tank (3) is sent into the first molecular sieve dehydration tower (2) and/or the second molecular sieve dehydration tower (2 ') through the second pipeline and/or the fourth pipeline for recycling;
the bottom of the gas-liquid phase separation tank (3) is connected with a liquid phase pipeline inlet of the rectifying tower (1) and is used for sending the water-containing dimethyl sulfoxide solution separated from the gas-liquid phase separation tank (3) to the rectifying tower (1) for retreatment.
2. The molecular sieve dehydration system for dimethyl sulfoxide according to claim 1 further comprising a reboiler (4), a condensing heat exchanger (5), a second condensing heat exchanger (5 '), a heater (6), a second heater (6'), a seventh valve (7), an eighth valve (7 '), a moisture detector (8) and a second moisture detector (8');
the reboiler (4) is connected to the bottom of the rectifying tower (1) and is used for heating and rectifying the aqueous dimethyl sulfoxide solution in the rectifying tower (1);
the first molecular sieve dehydration tower (2) and the second molecular sieve dehydration tower (2 ') are respectively connected with a condensation heat exchanger (5) and a second condensation heat exchanger (5') and are used for transferring heat generated in the molecular sieve adsorption process in the molecular sieve dehydration tower;
a connecting pipeline between the nitrogen source and the first molecular sieve dehydration tower (2) and a second pipeline between the gas-liquid phase separation tank (3) and the first molecular sieve dehydration tower (2) are combined into a first nitrogen pipeline, and the heater (6) and a seventh valve (7) are arranged on the first nitrogen pipeline in parallel; a connecting pipeline between the nitrogen source and the second molecular sieve dehydration tower (2 ') and a fourth pipeline between the gas-liquid phase separation tank (3) and the second molecular sieve dehydration tower (2') are combined into a second nitrogen pipeline, and the second heater (6 ') and the eighth valve (7') are arranged on the second nitrogen pipeline in parallel;
the heater (6) and the second heater (6 ') are heated by steam or electricity and used for heating the nitrogen flowing through and then sending the nitrogen into the molecular sieve dehydration tower, and the seventh valve (7) and the eighth valve (7') are used for adjusting and controlling the unheated nitrogen flowing through to enter the molecular sieve dehydration tower so as to finally adjust the temperature of the nitrogen entering the molecular sieve dehydration tower; the moisture detector (8) and the second moisture detector (8) are respectively connected with the tops of the first molecular sieve dehydration tower (2) and the second molecular sieve dehydration tower (2') and used for detecting the water content in the dimethyl sulfoxide discharged from the tops of the molecular sieve dehydration towers.
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| CN202020209668.8U CN212560057U (en) | 2020-02-25 | 2020-02-25 | Molecular sieve dehydration system for dimethyl sulfoxide |
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| CN202020209668.8U CN212560057U (en) | 2020-02-25 | 2020-02-25 | Molecular sieve dehydration system for dimethyl sulfoxide |
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