CN112239454B - System and method for producing sulfolane - Google Patents
System and method for producing sulfolane Download PDFInfo
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- CN112239454B CN112239454B CN201910645119.7A CN201910645119A CN112239454B CN 112239454 B CN112239454 B CN 112239454B CN 201910645119 A CN201910645119 A CN 201910645119A CN 112239454 B CN112239454 B CN 112239454B
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- C07D333/00—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom
- C07D333/02—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings
- C07D333/46—Heterocyclic compounds containing five-membered rings having one sulfur atom as the only ring hetero atom not condensed with other rings substituted on the ring sulfur atom
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Abstract
The invention provides a system for producing sulfolane and a method for producing sulfolene. The system comprises a first stripping column having a sulfolane reflux inlet and a first liquid phase outlet in communication; a hydrogenation unit in communication with the first liquid phase outlet; and the second stripping tower is communicated with the outlet of the hydrogenation device, and is provided with a sulfolane reflux outlet and a second liquid phase outlet, and the sulfolane reflux outlet is communicated with the sulfolane reflux inlet. According to the invention, the sulfolane reflux outlet of the second stripping tower is communicated with the sulfolane reflux inlet of the first stripping tower, so that the sulfolene can be directly prepared in the first stripping tower after stripping, the increase of the concentration of sulfur dioxide in the hydrogenation liquid caused by the increase of the concentration of sulfur dioxide in the conveying process is avoided, and the service life of the hydrogenation catalyst in the subsequent hydrogenation process is prolonged.
Description
Technical Field
The invention relates to the technical field of desulfurization, in particular to a system and a method for producing sulfolane.
Background
Sulfolane is a non-protonic, strongly polar and water-soluble organic sulfur solvent, and has the advantages of good thermal stability, strong dissolving capacity, high selectivity, weak corrosion to equipment, low toxicity to human bodies and the like. Sulfolane is used in arene extraction, as well as in reaction solvent, gas purification, fatty acid fractionation, etc. and may be also used in polymer, chemical fiber industry, product recovery and other special purposes.
At present, the synthesis process of sulfolane adopts a sulfolene hydrogenation method, i.e. 1, 3-butadiene and sulfur dioxide react to generate sulfolene in the presence of a polymerization inhibitor, and then the sulfolene is catalytically hydrogenated to obtain the sulfolane. The process generally comprises four steps in actual production: a synthesis step, a desulfurization step, a hydrogenation step and a refining step. Wherein, the function of the desulfurization step is to remove the unreacted sulfur dioxide in the synthesis reaction process, reduce the concentration of the unreacted sulfur dioxide and prevent the catalyst from being poisoned, so as to be beneficial to the smooth operation of the hydrogenation reaction. At present, the processes of the desulfurization part of the sulfolene product mainly comprise stripping, flash evaporation, chemical method desulfurization and the like. From the viewpoint of material recovery, most of the sulfur dioxide in the sulfolene is separated and recovered by a flash evaporation method, and then the residual sulfur dioxide in the sulfolene is removed by blowing.
The sulfolane production technologies disclosed in patent documents GB1123533, JP2012158543 and CN 102020632 all include a sulfur dioxide stripping step. However, after the completion of the stripping, the preparation of the hydrogenation solution is not performed immediately, but the stripped sulfolene is sent to a buffer tank or a preparation kettle through a pipeline to prepare the hydrogenation solution. Sulfolene has a high freezing point and generally becomes a solid at temperatures below 65 ℃, so that the temperature needs to be kept above 65 ℃ during stripping and transportation. At a temperature of above 65 ℃, sulfolene is unstable in property, is easy to decompose, generates a large amount of sulfur dioxide, and thus the blowing effect is greatly reduced. After the hydrogenation liquid is prepared, the freezing point of the hydrogenation liquid is lower than that of the sulfolene, so the hydrogenation liquid is prepared firstly, and then the stripping and conveying can be carried out at a lower temperature, so that the decomposition of the sulfolene is inhibited. However, the solubility of sulfur dioxide in sulfolane is much higher than that of sulfolene, which makes the difficulty of stripping hydrogenated liquid much higher than that of stripping sulfolane, and usually a method of high temperature, negative pressure or increasing gas-liquid ratio is used for stripping, so the scheme of preparing hydrogenated liquid first and then stripping brings about greater energy consumption and material consumption loss.
Disclosure of Invention
The invention mainly aims to provide a system and a method for producing sulfolane, which aim to solve the problems of low service life of a hydrogenation catalyst and large energy and material consumption loss in the prior art.
In order to achieve the above object, according to one aspect of the present invention, there is provided a system for producing sulfolane, comprising: a first stripping column having a sulfolane reflux inlet and a first liquid phase outlet in communication; a hydrogenation unit in communication with the first liquid phase outlet; and the second stripping tower is communicated with the outlet of the hydrogenation device, and is provided with a sulfolane reflux outlet and a second liquid phase outlet, and the sulfolane reflux outlet is communicated with the sulfolane reflux inlet.
Further, the inside batching mixed zone that is equipped with of first blowing tower, first liquid phase export and batching mixed zone intercommunication, sulfolane backward flow entry and batching mixed zone intercommunication.
Further, the first stripping tower is also provided with a water replenishing pipeline which is communicated with the ingredient mixing area.
Further, the first stripping tower is also provided with a first gas phase outlet, the second stripping tower is also provided with a second gas phase outlet, the system also comprises a tail gas pipeline, and the first gas phase outlet and the second gas phase outlet are respectively communicated with the tail gas pipeline.
Further, the system further comprises: the crude sulfolene synthesis device is communicated with the first blow-off tower and is used for providing crude sulfolene to be blown off to the first blow-off tower; and the sulfolane post-treatment device is connected with the second liquid phase outlet.
According to another aspect of the present invention, there is provided a process for producing sulfolene comprising the steps of: s1, carrying out primary air stripping treatment on the crude sulfolene to obtain a first solution containing the sulfolene, and preparing a hydrogenation liquid, wherein the hydrogenation liquid comprises the first solution; s2, carrying out hydrogenation treatment on the hydrogenated liquid to obtain a second solution containing crude sulfolane; s3, carrying out secondary stripping treatment on the second solution to obtain a third solution containing sulfolane, and refluxing part of the third solution serving as a reflux liquid to the step S1 for preparing a hydrogenation liquid.
Further, in step S1, the mass percentage of sulfur dioxide in the crude sulfolene is 0.5% to 1.5%.
Further, in the step S1, the stripping temperature of the first stripping treatment is 65 to 70 ℃, and the preferred stripping gas-liquid mass ratio is 1:10 to 1: 20.
Further, in step S1, the stripping temperature of the second stripping treatment is 55 to 65 ℃, the stripping pressure is preferably 30 to 45kPa, and the stripping gas-liquid mass ratio is more preferably 1:10 to 1: 20.
Further, in step S3, the reflux liquid is mixed with water to obtain a hydrogenated liquid, and the hydrogenated liquid is added to the first solution.
Furthermore, the mass percent of water in the hydrogenation liquid is 5-15%, and the mass ratio of the sulfolene to the sulfolane in the hydrogenation liquid is 1.5: 1-1: 1.
Further, in step S1, performing a first stripping treatment in a first stripping tower, wherein a blending material mixing area is arranged inside the first stripping tower; in step S3, the reflux liquid and water are introduced into the blending mixing zone to obtain a hydrogenated liquid.
According to the technical scheme, the system for producing the sulfolane comprises the first stripping tower, the hydrogenation device and the second stripping tower which are sequentially communicated, and the sulfolane reflux outlet of the second stripping tower is communicated with the sulfolane reflux inlet of the first stripping tower, so that the sulfolene can be directly prepared in the first stripping tower after stripping, the increase of the concentration of sulfur dioxide in the hydrogenation liquid caused by the increase of the concentration of sulfur dioxide in the conveying process is avoided, and the service life of a hydrogenation catalyst in the subsequent hydrogenation process is prolonged. In addition, the sulfolane used in the preparation of the hydrogenation liquid in the first stripping tower is the sulfolane blown by the second stripping tower instead of the sulfolane after post-treatment, so that the energy consumption and material consumption are saved, and the production cost is reduced. Furthermore, because the sulfolene in the hydrogenation liquid is inevitably subjected to decomposition reaction in the hydrogenation process to generate sulfur dioxide, a stripping tower needs to be arranged behind the hydrogenation device, and the second stripping tower adopted by the invention only advances the stripping device in the post-treatment device of the original sulfolane production process, so that the cost is not increased.
By applying the technical scheme provided by the invention, the sulfur dioxide content in the hydrogenation liquid can be reduced to 10 ppm-30 ppm, and the minimum consumption of the hydrogenation catalyst reaches 0.75%. Meanwhile, the device can realize continuous operation and is safe and reliable.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention. In the drawings:
FIG. 1 is a schematic diagram of a system for producing sulfolane according to an embodiment of the present invention;
fig. 2 is a schematic flow diagram of a process for producing sulfolane according to an embodiment of the present invention.
Wherein the figures include the following reference numerals:
1. a first stripping column; 2. a second stripping column; 3. a hydrogenation unit; 4. a first delivery pump; 5. a second delivery pump; 6. a fan; 7. a first liquid phase inlet; 8. a first gas phase inlet; 9. a first liquid phase outlet; 10. a first gas phase outlet; 11. a sulfolane reflux inlet; 13. a second liquid phase inlet; 14. a second gas phase inlet; 15. a second liquid phase outlet; 16. a second gas phase outlet; 18. a tail gas line; 19. a dosing line; 20. an output line; 21. a water replenishing pipeline; 22. an ingredient mixing zone.
Detailed Description
It should be noted that the embodiments and features of the embodiments may be combined with each other without conflict. The present invention will be described in detail below with reference to the embodiments with reference to the attached drawings.
In order to make those skilled in the art better understand the technical solutions of the present invention, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
It should be noted that the terms "first," "second," and the like in the description and claims of the present invention and in the drawings described above are used for distinguishing between similar elements and not necessarily for describing a particular sequential or chronological order. It should be understood that the data so used may be interchanged as appropriate in order to facilitate the embodiments of the invention described herein. Furthermore, the terms "comprises," "comprising," and "having," and any variations thereof, are intended to cover a non-exclusive inclusion, such that a process, method, system, article, or apparatus that comprises a list of steps or elements is not necessarily limited to those steps or elements expressly listed, but may include other steps or elements not expressly listed or inherent to such process, method, article, or apparatus.
As described in the background, the prior art processes for producing sulfolane have problems of low life of the hydrogenation catalyst, inconvenience of continuous operation, and large loss of energy and material consumption. The inventors of the present application studied in view of the above problems and proposed a system for producing sulfolane, as shown in fig. 1, comprising a first stripping column 1, a hydrogenation apparatus 3 and a second stripping column 2, the first stripping column 1 having a sulfolane reflux inlet 11 and a first liquid phase outlet 9 which are communicated; the hydrogenation device 3 is communicated with a first liquid phase outlet 9; the second stripping tower 2 is communicated with an outlet of the hydrogenation device 3, the second stripping tower 2 is provided with a sulfolane reflux outlet and a second liquid phase outlet 15, and the sulfolane reflux outlet is communicated with a sulfolane reflux inlet 11.
According to the invention, the sulfolane reflux outlet of the second stripping tower is communicated with the sulfolane reflux inlet of the first stripping tower, so that sulfur dioxide generated in the hydrogenation process is removed from sulfolene after stripping, and the preparation of the hydrogenation liquid can be directly carried out in the first stripping tower through a direct reflux mode, and the hydrogenation liquid can directly enter a hydrogenation device for hydrogenation, so that the increase of the concentration of sulfur dioxide in the hydrogenation liquid caused by the increase of the concentration of sulfur dioxide in the transportation process of sulfolene used for preparing the hydrogenation liquid in the prior art is avoided, and the service life of a hydrogenation catalyst in the subsequent hydrogenation process is prolonged.
And the sulfolane used in the preparation of the hydrogenation liquid in the first stripping tower is the sulfolane blown by the second stripping tower instead of the sulfolane after post-treatment, so that the energy consumption and material consumption are saved, and the production cost is reduced.
Furthermore, because the sulfolene in the hydrogenation liquid is inevitably subjected to decomposition reaction in the hydrogenation process to generate sulfur dioxide, a stripping tower needs to be arranged behind the hydrogenation device, and the second stripping tower adopted by the invention only advances the stripping device in the post-treatment device of the original sulfolane production process, so that the cost is not increased.
In the above system of the present invention, the second liquid phase outlet 15 of the second stripping column 2 and the sulfolane reflux outlet may be the same outlet, and are connected to the second transfer pump 5 by the same pipeline, and are separated after passing through the second transfer pump 5 and connected to the output pipeline 20 and the ingredient pipeline 19, respectively.
In the above system of the present invention, it is preferable that the first stripping tower 1 is provided therein with a material mixing zone 22, the first liquid phase outlet 9 is communicated with the material mixing zone 22, and the sulfolane reflux inlet 11 is communicated with the material mixing zone 22, as shown in fig. 1. More preferably, the first stripping column 1 further comprises a water replenishing line 21, and the water replenishing line 21 is communicated with the ingredient mixing zone 22, as shown in fig. 1.
In the prior art, the blown sulfolene generally needs to be sent to a buffer tank or a preparation kettle for preparation of a hydrogenation liquid, but the sulfolene has a high freezing point and generally becomes a solid state below 65 ℃, so the temperature needs to be kept above 65 ℃ in the blowing and conveying processes, and when the temperature is above 65 ℃, the sulfolene is unstable in property and is easy to decompose to generate a large amount of sulfur dioxide, so the blowing effect is greatly reduced. According to the invention, by arranging the material mixing area 22, part of the treatment liquid passing through the second stripping tower 2 is directly subjected to liquid distribution in the material mixing area 22 after flowing back to the first stripping tower 1, so that the decomposition of the sulfolene in the conveying process is avoided, and the stripping effect is improved.
In the above system of the present invention, as shown in fig. 1, the first stripping tower 1 further has a first gas phase outlet 10, and the second stripping tower 2 further has a second gas phase outlet 16, and preferably, the system further includes a tail gas line 18, and the first gas phase outlet 10 and the second gas phase outlet 16 are respectively communicated with the tail gas line.
The system of the present invention further comprises a crude sulfolene synthesis unit and a sulfolane post-treatment unit. The crude sulfolene synthesis device is used for synthesizing crude sulfolene, and the sulfolane post-treatment device can be used for storing the obtained sulfolane and recycling the tail gas and the like. The crude sulfolene synthesis device is communicated with the first stripping tower 1 and is used for providing crude sulfolene to be stripped to the first stripping tower 1; the sulfolane post-treatment device is connected to the second liquid phase outlet 15.
According to another aspect of the present invention, there is also provided a method for producing sulfolene, as shown in fig. 2, comprising the steps of: s1, carrying out primary stripping treatment (primary stripping as shown in figure 2) on the crude sulfolene to obtain a first solution containing the sulfolene, and preparing a hydrogenation liquid, wherein the hydrogenation liquid comprises the first solution; s2, carrying out hydrogenation treatment on the hydrogenated liquid to obtain a second solution containing crude sulfolane; s3, performing a second stripping treatment (such as the second stripping shown in fig. 2) on the second solution to obtain a third solution containing sulfolane, and refluxing a part of the third solution as a reflux liquid to the step S1 for preparing a hydrogenated liquid.
According to the method, the sulfolane obtained through the stripping treatment is refluxed to the step S1 to prepare the hydrogenation liquid, so that the increase of the sulfur dioxide concentration in the hydrogenation liquid caused by the increase of the sulfur dioxide concentration in the conveying process is avoided, and the service life of the hydrogenation catalyst in the subsequent hydrogenation process is prolonged. In addition, the sulfolane obtained by the secondary blowing treatment of the fine process used in the process of preparing the hydrogenation liquid is not the product sulfolane after post treatment, so that the energy consumption and material consumption are saved, and the production cost is reduced.
In the step S1, the mass percentage of the sulfur dioxide in the crude sulfolene is preferably 0.5% to 1.5%. The stripping temperature of the first stripping treatment is 65-70 ℃, and the mass ratio of stripping gas to liquid is 1: 10-1: 20.
In the step S3, it is preferable that the stripping temperature of the second stripping process is 55 to 65 ℃, the stripping pressure is 30 to 45kPa, and the stripping gas-liquid mass ratio is 1:10 to 1: 20.
In the above step S3, the second stripping treatment yields a third solution containing sulfolane, a part of the third solution containing sulfolane is mixed with water as a reflux liquid to yield a hydrogenated liquid, and the hydrogenated liquid is added to the first solution. In this case, the hydrogenated liquid includes sulfolene obtained through the first blow-off treatment, a part of sulfolane obtained through the second blow-off treatment, and water, and preferably, in the hydrogenated liquid, the mass percentage of water is 5% to 15%, and the mass ratio of sulfolene to sulfolane is 1.5:1 to 1: 1. And carrying out post-treatment on the other part of the sulfolane obtained after the second air stripping treatment to obtain a sulfolane product.
In the step S1, the first blown-off tail gas obtained after the first blowing of the crude sulfolene is performed, and in the step S2, the second blown-off tail gas obtained after the second blowing of the second solution containing the crude sulfolane is performed, at this time, the first blown-off tail gas and the second blown-off tail gas may be subjected to tail gas treatment, so as to reduce environmental pollution.
In order to improve the stripping effect, in a preferred embodiment, in step S1, the first stripping treatment is performed in a first stripping tower, and an ingredient mixing area is arranged inside the first stripping tower; in the step S3, the reflux liquid and water are introduced into the blending mixing area to obtain the hydrogenated liquid.
Specifically, the above-described process for producing sulfolene according to the present invention may employ the above-described system for producing sulfolane, as shown in fig. 1, when the process comprises the steps of:
crude sulfolene enters a first stripping tower 1 through a first stripping tower liquid phase inlet 7, air enters the first stripping tower 1 through a first stripping tower gas phase inlet 8, the first stripping tower 1 is a normal pressure stripping tower, the air and the first stripping tower 1 are in gas-liquid contact in the first stripping tower 1 to complete a stripping process, first stage stripping tail gas enters a tail gas pipeline 18 through a first stripping tower gas phase outlet 10, the sulfolene obtained after stripping descends to a batching mixing zone 22 of the first stripping tower 1, the sulfolene obtained by stripping in a second stripping tower 2 is mixed with water entering through a water supplementing pipeline 21 to prepare hydrogenation liquid, and the obtained hydrogenation liquid is discharged through a first stripping tower liquid phase outlet 9 and enters a first conveying pump 4;
the hydrogenation liquid enters a hydrogenation device 3 through a first delivery pump 4 for hydrogenation, crude sulfolane is obtained after hydrogenation, and the crude sulfolane enters a second stripping tower 2 through an outlet of the hydrogenation device 4;
crude sulfolane gets into second air stripping tower 2 through the liquid phase entry 13 of second air stripping tower 2, air gets into second air stripping tower 2 through the gaseous phase entry 14 of second air stripping tower 2, second air stripping tower 2 is the decompression air stripping tower, the two carries out gas-liquid contact in second air stripping tower 2, accomplish the air stripping process, second level air stripping tail gas passes through the gaseous phase export 16 of second air stripping tower 2 and sends out second air stripping tower 2, then gets into tail gas pipeline 18 through fan 6, the sulfolane obtained after the air stripping discharges through the liquid phase export 15 of second air stripping tower 2, get into second delivery pump 5, a part of sulfolane is sent out by second delivery pump 5, another part is sent to the batching mixed zone 22 of first air stripping tower 1 through batching pipeline 19 by second delivery pump 5 and participates in the preparation of hydrogenation liquid.
The system and method for producing sulfolane according to the present invention will be further illustrated with reference to the following examples.
The following examples all adopt the structure as shown in fig. 1 for the system for producing sulfolane, and the first stripping tower liquid phase inlet links to each other with sulfolene flash distillation plant, and the export pipeline links to each other with sulfolane aftertreatment device, and the tail gas pipeline links to each other with tail gas treatment device.
The processes for producing sulfolane in the following examples all use the flow scheme shown in fig. 2, and the crude sulfolane comes from a sulfolane flash distillation plant, and the first stage tail gas and the second stage tail gas are both sent to a tail gas treatment plant through a tail gas pipeline 18, and the sulfolane sent by the second transfer pump 5 is sent to a sulfolane post-treatment plant.
Example 1
This example employed the apparatus configuration shown in FIG. 1 and the operation scheme shown in FIG. 2, wherein the stripping temperature of the first stripping column 1 was 68 ℃ and the stripping gas-liquid ratio was 1: 10. The stripping temperature of the second stripping tower 2 is 60 ℃, the stripping pressure is 40kPa, and the stripping gas-liquid ratio is 1: 10. The mass fraction of sulfur dioxide in the crude sulfolene was 0.7%. The mass fraction of water in the hydrogenation liquid is 10%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1: 1. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 13 ppm.
Example 2
This example employed the apparatus configuration shown in FIG. 1 and the operation scheme shown in FIG. 2, wherein the stripping temperature of the first stripping column 1 was 70 ℃ and the stripping gas-liquid ratio was 1: 15. The stripping temperature of the second stripping tower 2 is 55 ℃, the stripping pressure is 30kPa, and the stripping gas-liquid ratio is 1: 20. The mass fraction of sulfur dioxide in the crude sulfolene was 1.1%. The mass fraction of water in the hydrogenation liquid is 10%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1.5: 1. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 21 ppm.
Example 3
This example differs from example 1 in that: wherein the stripping temperature of the first stripping tower 1 is 65 ℃, and the stripping gas-liquid ratio is 1: 10. The concentration of sulfur dioxide in the finally obtained hydrogenation liquid is 15 ppm.
Example 4
This example differs from example 1 in that: the stripping temperature of the first stripping tower 1 is 70 ℃, and the stripping gas-liquid ratio is 1: 20. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 18 ppm.
Example 5
This example differs from example 1 in that: the stripping temperature of the second stripping tower 2 is 65 ℃, the stripping pressure is 45kPa, and the stripping gas-liquid ratio is 1: 10. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 19 ppm.
Example 6
This example differs from example 1 in that: the stripping temperature of the second stripping tower 2 is 55 ℃, the stripping pressure is 30kPa, and the stripping gas-liquid ratio is 1: 20. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 17 ppm.
Example 7
This example differs from example 1 in that: the mass fraction of water in the hydrogenation liquid is 5%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1: 1. The concentration of sulfur dioxide in the finally obtained hydrogenation liquid is 15 ppm.
Example 8
This example differs from example 1 in that: the mass fraction of water in the hydrogenation liquid is 15%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1.2: 1. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 12 ppm.
Example 9
The apparatus configuration shown in FIG. 1 and the operation scheme shown in FIG. 2 were employed, in which the stripping temperature of the first stripping column 1 was 60 ℃ and the stripping gas-liquid ratio was 1: 8. The stripping temperature of the second stripping tower 2 is 52 ℃, the stripping pressure is 50kPa, and the stripping gas-liquid ratio is 1: 8. The mass fraction of sulfur dioxide in the crude sulfolene was 0.7%. The mass fraction of water in the hydrogenation liquid is 3%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1: 1. The sulfur dioxide concentration in the finally obtained hydrogenation liquid is 27 ppm.
Example 10
The apparatus configuration shown in FIG. 1 and the operation scheme shown in FIG. 2 were employed, in which the stripping temperature of the first stripping column 1 was 70 ℃ and the stripping gas-liquid ratio was 1: 20. The stripping temperature of the second stripping tower 2 is 55 ℃, the stripping pressure is 40kPa, and the stripping gas-liquid ratio is 1: 20. The mass fraction of sulfur dioxide in the crude sulfolene was 0.7%. The mass fraction of water in the hydrogenation liquid is 15%, the balance is sulfolene and sulfolane, and the mass ratio of the sulfolene to the sulfolane is 1.2: 1. The concentration of sulfur dioxide in the finally obtained hydrogenation liquid is 20 ppm.
The above description is only exemplary of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
From the above description, it can be seen that the above-described embodiments of the present invention achieve the following technical effects:
1. the concentration of sulfur dioxide in the sulfolene hydrogenation liquid is effectively reduced, and the poisoning of a hydrogenation catalyst is prevented;
2. the use efficiency of the catalyst is improved, and the replacement frequency of the catalyst is reduced, so that the device can run for a long period; therefore, the consumption of the catalyst is reduced, the cost is saved, and the environment protection is facilitated;
3. the sulfolane used in the process of preparing the hydrogenation liquid is the sulfolane blown off by the second blow-off tower, and the sulfolane after post-treatment is not used, so that the energy consumption and material consumption are saved, and the production cost is reduced
4. The device can realize continuous operation, and is safe and reliable.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention.
Claims (8)
1. An apparatus for producing sulfolane, comprising:
a first stripping column (1) having a sulfolane reflux inlet (11) and a first liquid phase outlet (9) in communication;
a hydrogenation unit (3) in communication with the first liquid phase outlet (9);
a second stripping column (2) in communication with the outlet of the hydrogenation unit (3), the second stripping column (2) having a sulfolane reflux outlet in communication with the sulfolane reflux inlet (11) and a second liquid phase outlet (15);
a crude sulfolene synthesis device which is communicated with the first blow-off tower (1) and is used for providing crude sulfolene to be blown off to the first blow-off tower (1);
a sulfolane post-treatment device connected to the second liquid phase outlet (15); wherein the content of the first and second substances,
a material mixing area (22) is arranged in the first stripping tower (1), the first liquid phase outlet (9) is communicated with the material mixing area (22), and the sulfolane reflux inlet (11) is arranged on a shell corresponding to the material mixing area (22);
the first blow-drying tower (1) is also provided with a water replenishing pipeline (21), and the water replenishing pipeline (21) is communicated with the ingredient mixing area (22); the first stripping tower (1) is also provided with a first gas phase outlet (10), the second stripping tower (2) is also provided with a second gas phase outlet (16), the device further comprises a tail gas pipeline (18), and the first gas phase outlet (10) and the second gas phase outlet (16) are respectively communicated with the tail gas pipeline.
2. A method for producing sulfolane using the apparatus for producing sulfolane according to claim 1, comprising the steps of:
s1, carrying out primary stripping treatment on the crude sulfolene in a first stripping tower (1) to obtain a first solution containing the sulfolene, and preparing a hydrogenation liquid in a material mixing area (22) in the first stripping tower (1);
s2, carrying out hydrogenation treatment on the hydrogenated liquid in a hydrogenation device (3) to obtain a second solution containing crude sulfolane;
s3, performing secondary stripping treatment on the second solution in a second stripping tower (2) to obtain a third solution containing sulfolane, and refluxing a part of the third solution serving as a reflux liquid to the step S1 for preparing the hydrogenated liquid;
wherein the reflux liquid, water and the first solution are mixed to obtain the hydrogenation liquid; the mass percentage of water in the hydrogenation liquid is 5-15%, and the mass ratio of the sulfolene to the sulfolane in the hydrogenation liquid is 1.5: 1-1: 1.
3. The method of claim 2, wherein in step S1, the mass percent of sulfur dioxide in the crude sulfolene is 0.5% to 1.5%.
4. The method of claim 2 or 3, wherein in the step S1, the stripping temperature of the first stripping treatment is 65 ℃ to 70 ℃.
5. The method according to claim 2 or 3, wherein in the step S1, the mass ratio of stripping gas to liquid in the first stripping treatment is 1: 10-1: 20.
6. The method of claim 2, wherein in the step S3, the stripping temperature of the second stripping treatment is 55-65 ℃.
7. The method according to claim 6, wherein in the step S3, the blow-off pressure of the second blow-off treatment is 30kPa to 45 kPa.
8. The method according to claim 2, wherein in the step S3, the stripping gas-liquid mass ratio of the second stripping treatment is 1: 10-1: 20.
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