CN215781608U - Carbazole system of refining - Google Patents
Carbazole system of refining Download PDFInfo
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- CN215781608U CN215781608U CN202122223873.7U CN202122223873U CN215781608U CN 215781608 U CN215781608 U CN 215781608U CN 202122223873 U CN202122223873 U CN 202122223873U CN 215781608 U CN215781608 U CN 215781608U
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Abstract
The utility model provides a carbazole refining system, and belongs to the technical field of chemical separation. The carbazole refining system comprises a reduced pressure rectification unit and a recrystallization unit, wherein the reduced pressure rectification unit comprises a rectification tower and a residual liquid tank, a residual liquid discharge pipe is arranged at the bottom of the rectification tower, and a liquid discharge control valve is arranged on the residual liquid discharge pipe; the residual liquid discharge pipe is connected with an intermediate tank, the intermediate tank is arranged above the residual liquid tank, the bottom of the intermediate tank is provided with a liquid discharge pipe, the liquid discharge pipe is connected with the residual liquid tank, and the liquid discharge pipe is provided with a liquid discharge cut-off valve; the intermediate tank is provided with a negative pressure adjusting pipe fitting, and the negative pressure adjusting pipe fitting is provided with a negative pressure adjusting valve; still be provided with first nitrogen gas air supplement pipe on the pans, set up first nitrogen gas gulp valve on the first nitrogen gas air supplement pipe. When the residual liquid is discharged, the residual liquid is discharged into the intermediate tank, and then the residual liquid is discharged into the residual liquid tank through the intermediate tank, so that the smooth liquid discharge is ensured, the reverse suction of air is avoided, and the vacuum of the system is damaged.
Description
Technical Field
The utility model belongs to the technical field of chemical separation, and particularly relates to a carbazole refining system.
Background
Carbazole is a nitrogen-containing heterocyclic compound, is one of the most economic components in coal tar, 90% of carbazole in the world is obtained from coal tar, and carbazole can be used for producing dyes, pigments, photoconductors, photosensitive materials, special printing ink and the like.
A rectification method is adopted, a crude carbazole product with the purity of 85-90% can be separated and extracted from a mixed solution enriched with anthracene and carbazole, and the crude carbazole product can be recrystallized to prepare a refined carbazole product with the purity of more than 98.5%. In the prior art, when anthracene and carbazole are separated from mixed oil by adopting a vacuum rectification process, carbazole fraction is extracted from a side line of a rectification tower. When the residual liquid in the tower kettle is enriched to a certain liquid level, the residual liquid needs to be discharged to a residual liquid tank. However, the system is under negative pressure, so that the residual liquid is discharged smoothly or air is sucked backwards easily to destroy the vacuum of the system.
Disclosure of Invention
In view of this, the present invention provides a carbazole refining system to solve the technical problem of unsmooth discharge of residual liquid from a carbazole rectifying tower in the prior art.
The technical scheme adopted by the utility model for solving the technical problems is as follows:
a carbazole refining system comprises a reduced pressure rectification unit and a recrystallization unit, wherein the reduced pressure rectification unit comprises a rectification tower and a residual liquid tank, a residual liquid discharge pipe is arranged at the bottom of the rectification tower, and a liquid discharge control valve is arranged on the residual liquid discharge pipe; the residual liquid discharge pipe is connected with an intermediate tank, the intermediate tank is arranged above the residual liquid tank, the bottom of the intermediate tank is provided with a liquid discharge pipe, the liquid discharge pipe is connected with the residual liquid tank, and a liquid discharge cut-off valve is arranged on the liquid discharge pipe; a negative pressure adjusting pipe fitting is arranged on the intermediate tank, and a negative pressure adjusting valve is arranged on the negative pressure adjusting pipe fitting; still be provided with first nitrogen gas air supplement pipe on the pans, set up first nitrogen gas gulp valve on the first nitrogen gas air supplement pipe.
As a further description of the above technical solution:
and a liquid level sensor is arranged on the rectifying tower and electrically connected with the negative pressure regulating valve.
As a further description of the above technical solution:
the lateral line of rectifying column is connected with the carbazole condenser, carbazole fraction jar is connected to the lime set discharge end of carbazole condenser, the discharge end of carbazole fraction jar is provided with the carbazole bleeder pump, the discharge end of carbazole bleeder pump is connected the recrystallization unit.
As a further description of the above technical solution:
the discharge end of the carbazole discharge pump is connected with a crude carbazole mixing and dissolving tank, the discharge end of the crude carbazole mixing and dissolving tank is connected with the recrystallization unit, and the feed end of the crude carbazole mixing and dissolving tank is also connected with a first solvent feed pipe.
As a further description of the above technical solution:
the recrystallization unit comprises a recrystallization tank, wherein a suction filtration filtrate discharging pipe is arranged at the bottom of the recrystallization tank and connected with the residual liquid tank.
As a further description of the above technical solution:
a stirrer is arranged in the recrystallization tank; a suction filter plate is arranged at the bottom of the recrystallization tank, and a suction filter cavity is formed between the suction filter plate and the bottom of the recrystallization tank; the bottom of recrystallization jar still is provided with the second solvent inlet pipe, solvent feed pipe spare intercommunication the suction filtration chamber.
As a further description of the above technical solution:
the top of recrystallization jar is provided with negative pressure extraction pipe and second nitrogen air supplement pipe, be provided with first shut-off valve on the negative pressure extraction pipe, be provided with the second trip valve on the second nitrogen air supplement pipe.
As a further description of the above technical solution:
the wall of the recrystallization tank is provided with a heat exchange jacket, the lower end of the heat exchange jacket is connected with a cold medium feeding pipe, the upper end of the heat exchange jacket is connected with a cold medium discharging pipe, the cold medium feeding pipe is provided with a third stop valve, and the cold medium discharging pipe is provided with a fourth stop valve.
As a further description of the above technical solution:
the lower end of the heat exchange jacket is also connected with a heat medium feeding pipe, the upper end of the heat exchange jacket is also connected with a heat medium discharging pipe, a fifth stop valve is arranged on the heat medium feeding pipe, and a sixth stop valve is arranged on the heat medium discharging pipe.
According to the technical scheme, the utility model provides a carbazole refining system, which has the beneficial effects that: set up the pans at the bottom discharge end of the tower that is used for refining the rectifying column of carbazole, work as when rectifying column tower cauldron raffinate is enriched to certain liquid level, through the pipe fitting is adjusted to the negative pressure, makes be the negative pressure in the pans, then opens drainage control valve carries out the flowing back, and it is smooth and easy to guarantee the flowing back, avoids the air suck-back, destroys the system vacuum. After the flowing back is ended, close negative pressure governing valve and drainage control valve, open flowing back trip valve first nitrogen gas gulp valve to let in nitrogen gas in the pans, make the gas phase space of pans is ordinary pressure or malleation, with to smoothly unload in the residual liquid jar, also can pass through first nitrogen gas gulp pipe, will the raffinate material in the pans is pressed extremely in the residual liquid jar, improves the speed of unloading.
Drawings
FIG. 1 is an apparatus flow diagram of a carbazole refining system.
In the figure: the system comprises a carbazole refining system 10, a rectifying tower 100, a raffinate discharge pipe 110, a liquid discharge control valve 111, an oil-mixed feeding pipe 120, a reboiler 130, a first condenser 141, a first fraction tank 142, a first discharge pump 143, a carbazole condenser 151, a carbazole fraction tank 152, a carbazole discharge pump 153, a residual liquid tank 200, an intermediate tank 300, a liquid discharge pipe 310, a liquid discharge shut-off valve 311, a negative pressure adjusting pipe 320, a negative pressure adjusting valve 321, a first nitrogen gas supply pipe 330, a first nitrogen gas supply valve 331, a crude carbazole miscible tank 400, a first solvent feeding pipe 410, a recrystallization tank 500, a suction filtration filtrate discharging pipe 510, a stirrer 520, a suction filtration plate 530, a suction filtration cavity 540, a second solvent feeding pipe 550, a solvent feeding control valve 551, a negative pressure extraction pipe 560, a first cut-off valve 561, a second nitrogen gas supply pipe 570, a second cut-off valve 571, a crude carbazole solution feeding pipe 580, a crude carbazole feeding control valve 581, a heat exchange jacket 600, a liquid-mixed feeding pipe 120, a reboiler 130, a first condenser 141, a first nitrogen gas supply pipe 330, a second nitrogen gas supply pipe, a second solvent supply pipe, a second solvent, a second solvent, a second, a third, cold medium feed pipe 610, third shut-off valve 611, cold medium discharge pipe 620, fourth shut-off valve 621, heat medium feed pipe 630, fifth shut-off valve 631, heat medium discharge pipe 640, sixth shut-off valve 641.
Detailed Description
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.
Referring to fig. 1, in an embodiment, a carbazole refining system 10 includes a vacuum rectification unit and a recrystallization unit, the vacuum rectification unit includes a rectification tower 100 and a residue tank 200, a residue discharge pipe 110 is disposed at a bottom of the rectification tower 100, and a liquid discharge control valve 111 is disposed on the residue discharge pipe 110. The residual liquid discharge pipe 110 is connected with an intermediate tank 300, the intermediate tank 300 is arranged above the residual liquid tank 200, the bottom of the intermediate tank is provided with a liquid discharge pipe 310, the liquid discharge pipe 310 is connected with the residual liquid tank 200, and the liquid discharge pipe 310 is provided with a liquid discharge cut-off valve 311. The intermediate tank 300 is provided with a negative pressure adjusting pipe 320, and the negative pressure adjusting pipe 320 is provided with a negative pressure adjusting valve 321. The intermediate tank 300 is further provided with a first nitrogen gas supplementing pipe 330, and the first nitrogen gas supplementing pipe 330 is provided with a first nitrogen gas supplementing valve 331.
When the raffinate in the bottom of the rectifying tower 100 is enriched to a certain level, the interior of the intermediate tank 300 is made to be at a negative pressure through the negative pressure adjusting pipe 320, and then the drainage control valve 111 is opened to drain the liquid. During liquid drainage, as the pressure in the intermediate tank 300 is negative and is equal to or slightly higher than the pressure in the rectifying tower 100, the residual liquid ensures smooth liquid drainage under the action of gravity, and prevents air from being sucked backwards to damage the vacuum of the system.
After the liquid drainage is finished, the negative pressure regulating valve 321 and the liquid drainage control valve 111 are closed, the liquid drainage cut-off valve 311 and the first nitrogen gas supplementing valve 331 are opened, nitrogen gas is introduced into the intermediate tank 300, so that the gas phase space of the intermediate tank is at normal pressure or positive pressure, the material can be smoothly discharged from the residual liquid tank 200, and the material can be pressed into the residual liquid tank 200 through the first nitrogen gas supplementing pipe 330, so that the discharging speed is improved.
In a specific embodiment, an oil mixing feeding pipe fitting 120 is disposed at the feeding end of the rectifying tower 100, and is used for feeding the mixed oil enriched with anthracene, phenanthrene and carbazole components into the rectifying tower 100. The tower bottom of the rectifying tower 100 is provided with a reboiler 130 for heating the material in the rectifying tower 100. The top of rectifying column 100 is provided with anthracene phenanthrene fraction and adopts the subassembly, including connecting the first condenser 141 of rectifying column top of the tower, connecting the first fraction jar 142 and the setting of the lime set discharge end of first condenser 141 are in the first discharge pump 143 of first fraction jar bottom. The anthracene-phenanthrene fraction extraction assembly is used for extracting anthracene and phenanthrene mixtures.
The lateral line of rectifying column 100 is provided with carbazole fraction and takes out the subassembly, including connecting the carbazole condenser 151 of rectifying column lateral part, carbazole fraction jar 152 is connected to the lime set discharge end of carbazole condenser 151, the discharge end of carbazole fraction jar 152 is provided with carbazole bleeder pump 153, the discharge end of carbazole bleeder pump 153 is connected the recrystallization unit. The carbazole fraction extraction component is used for extracting carbazole fraction.
The gas phase outlets of the first condenser 141 and the carbazole condenser 151 are connected with a negative pressure control pipe fitting 160 to realize the vacuum rectification.
In a preferred embodiment, the rectifying tower 100 is provided with a liquid level sensor, and the liquid level sensor is electrically connected to the negative pressure regulating valve 321. During normal production, the negative pressure regulating valve 321 is closed, the intermediate tank 300 maintains normal pressure or negative pressure, and when the liquid level of the raffinate in the rectifying tower 100 is enriched to a target liquid level, the negative pressure regulating valve 321 firstly acts to regulate the pressure in the intermediate tank 300 to be negative pressure, and the negative pressure is equal to or slightly less than the pressure at the top of the rectifying tower 100. Then the drainage control valve 111 acts to drain the liquid normally, so that automatic drainage is realized, and the operation risk is reduced.
In one embodiment, the discharge end of the carbazole discharge pump 153 is connected to a crude carbazole miscible tank 400, the discharge end of the crude carbazole miscible tank 400 is connected to the recrystallization unit, and the feed end of the crude carbazole miscible tank 400 is further connected to a first solvent feed pipe 410. The crude carbazole fraction is pumped into the crude carbazole miscible tank 400 for temporary storage, and in order to prevent crystallization, a solvent is introduced into the crude carbazole miscible tank 400 through the first solvent feeding pipe 410, and the tank temperature of the crude carbazole miscible tank 400 is maintained at a higher temperature.
In one embodiment, the recrystallization unit comprises a recrystallization tank 500, a suction filtrate discharge pipe 510 is arranged at the bottom of the recrystallization tank 500, and the suction filtrate discharge pipe 510 is connected with the residual liquid tank 200. When the residual liquid in the tower bottom is enriched to a certain liquid level, the residual liquid is discharged to a residual liquid tank 200, and the carbazole component with a certain concentration also exists in the residual liquid. Meanwhile, in the recrystallization process, the filtrate of the suction filtration also carries part of carbazole components. And mixing the solvent generated in the recrystallization process with the rectification residual liquid, and further extracting the carbazole component through the processes of primary solvent crystallization, rectification and secondary solvent crystallization, thereby improving the yield of carbazole.
Preferably, a stirrer 520 is arranged in the recrystallization tank 500, a suction filter plate 530 is arranged at the bottom of the recrystallization tank 500, and a suction filter cavity 540 is formed between the suction filter plate 530 and the bottom of the recrystallization tank 500. The bottom of the recrystallization tank 500 is provided with a second solvent feeding pipe 550, and the second solvent feeding pipes 550 are respectively communicated with the filtration cavity 540.
In this embodiment, the carbazole crystal after at least one recrystallization is placed in the recrystallization tank 500, and when the next recrystallization is required, the valve on the filtrate discharge pipe 510 is closed, and the valve on the second solvent feed pipe 550 is opened to feed the solvent into the filtration chamber 540. Under the action of pressure, the solvent permeates through the filter plate 530 and gradually permeates upward from the bottom of the carbazole crystals, so that the crystals at the bottom gradually dissolve, and the crystals at the upper part loosen under the action of gravity, thereby facilitating the quick start of the stirrer 520. Therefore, after each recrystallization, the liquid phase in the recrystallization tank 500 can be completely drained, so that the recrystallization times are reduced, the solvent dosage is reduced, the solvent use efficiency is improved, and the carbazole yield is improved. Meanwhile, the degree of each suction filtration does not need to be controlled, so that the operation difficulty is greatly reduced.
Preferably, in order to improve the feeding efficiency and the disturbance degree of the carbazole crystals, a negative pressure extraction pipe 560 and a second nitrogen supplementary pipe 570 are arranged at the top of the recrystallization tank 500, a first cut-off valve 561 is arranged on the negative pressure extraction pipe 560, and a second cut-off valve 571 is arranged on the second nitrogen supplementary pipe 570. When the solvent is fed from the bottom of the recrystallization tank 500, the first cut-off valve 561 is opened, and the second cut-off valve 571 is closed, so that the gas phase space of the recrystallization tank 500 is at a negative pressure, thereby accelerating the upward permeation of the solvent and rapidly slurrying the carbazole crystals. In the recrystallization process, the first shut-off valve 561 is closed, and the second shut-off valve 571 is opened, so that the gas phase space of the recrystallization tank 500 is returned to normal pressure. Preferably, in order to accelerate the suction filtration process and improve the suction filtration effect, the second cut-off valve 571 can be opened during suction filtration, so that the gas phase space of the recrystallization tank 500 has a certain pressure.
In one embodiment, the second solvent feeding pipe 550 is provided with a solvent feeding control valve 551 to control the feeding rate and feeding amount of the solvent.
In yet another embodiment, the top of the recrystallization tank 500 is provided with a crude carbazole solution feed pipe 580, and the crude carbazole solution feed pipe 580 is provided with a crude carbazole feed control valve 581. When the recrystallization tube 200 is fed for the first time, crude carbazole and a solvent may be mixed in advance to form a mixture, and then the mixture is fed into the recrystallization tank 500 through the crude carbazole solution feeding tube 580, so that the feeding efficiency is improved, and the operation process is optimized.
In a preferred embodiment, a heat exchange jacket 600 is disposed on the wall of the recrystallization tank 500, a cold medium feeding pipe 610 is connected to the lower end of the heat exchange jacket 600, a cold medium discharging pipe 620 is connected to the upper end of the heat exchange jacket, a third cut-off valve 611 is disposed on the cold medium feeding pipe, and a fourth cut-off valve 621 is disposed on the cold medium discharging pipe. In the recrystallization process, a cooling medium, such as circulating water, cooling water, etc., is introduced into the heat exchange jacket 600 to control the cooling rate and improve the recrystallization effect.
Further, the lower end of the heat exchange jacket 600 is further connected with a heat medium feeding pipe 630, the upper end of the heat exchange jacket is further connected with a heat medium discharging pipe 640, the heat medium feeding pipe 630 is provided with a fifth cut-off valve 631, and the heat medium discharging pipe 640 is provided with a sixth cut-off valve 641. In the process of adding the solvent into the recrystallization tank 500 from the bottom of the recrystallization tank 500, a heat medium, such as hot water, boiler water, steam, etc., is introduced into the heat exchange jacket 600 to increase the temperature in the recrystallization tank 500 and increase the dissolution rate of the solvent to carbazole.
In one embodiment, the stirrer 520 is a gate stirrer to improve stirring effect.
In yet another embodiment, the suction filter plate 530 is a sintered plate.
Finally, it should be noted that: although the present invention has been described in detail with reference to the foregoing embodiments, it will be apparent to those skilled in the art that modifications may be made to the embodiments or portions thereof without departing from the spirit and scope of the utility model.
Claims (9)
1. A carbazole refining system comprises a reduced pressure rectification unit and a recrystallization unit, and is characterized in that the reduced pressure rectification unit comprises a rectification tower and a residual liquid tank, a residual liquid discharge pipe is arranged at the bottom of the rectification tower, and a liquid discharge control valve is arranged on the residual liquid discharge pipe; the residual liquid discharge pipe is connected with an intermediate tank, the intermediate tank is arranged above the residual liquid tank, the bottom of the intermediate tank is provided with a liquid discharge pipe, the liquid discharge pipe is connected with the residual liquid tank, and a liquid discharge cut-off valve is arranged on the liquid discharge pipe; a negative pressure adjusting pipe fitting is arranged on the intermediate tank, and a negative pressure adjusting valve is arranged on the negative pressure adjusting pipe fitting; still be provided with first nitrogen gas air supplement pipe on the pans, set up first nitrogen gas gulp valve on the first nitrogen gas air supplement pipe.
2. The carbazole refining system according to claim 1, wherein a liquid level sensor is disposed on the rectifying tower, and the liquid level sensor is electrically connected to the negative pressure regulating valve.
3. The carbazole refining system according to claim 1, wherein a carbazole condenser is connected to a side line of the rectifying tower, a condensate discharge end of the carbazole condenser is connected to a carbazole fraction tank, a carbazole discharge pump is disposed at a discharge end of the carbazole fraction tank, and a discharge end of the carbazole discharge pump is connected to the recrystallization unit.
4. The carbazole refining system according to claim 3, wherein a discharge end of the carbazole discharge pump is connected to a crude carbazole miscible tank, a discharge end of the crude carbazole miscible tank is connected to the recrystallization unit, and a feed end of the crude carbazole miscible tank is further connected to a first solvent feed pipe.
5. The carbazole refining system according to claim 1, wherein the recrystallization unit includes a recrystallization tank, and a suction filtrate discharge pipe is provided at a bottom of the recrystallization tank, and the suction filtrate discharge pipe is connected to the residual liquid tank.
6. The carbazole refining system according to claim 5, wherein an agitator is provided in the recrystallization tank; a suction filter plate is arranged at the bottom of the recrystallization tank, and a suction filter cavity is formed between the suction filter plate and the bottom of the recrystallization tank; the bottom of recrystallization jar still is provided with the second solvent inlet pipe, solvent feed pipe spare intercommunication the suction filtration chamber.
7. The carbazole refining system according to claim 6, wherein a negative pressure extraction pipe and a second nitrogen supply pipe are provided at a top of the recrystallization tank, the negative pressure extraction pipe is provided with a first cut-off valve, and the second nitrogen supply pipe is provided with a second cut-off valve.
8. The carbazole refining system according to claim 6, wherein a heat exchange jacket is provided on a tank wall of the recrystallization tank, a cold medium feed pipe is connected to a lower end of the heat exchange jacket, a cold medium discharge pipe is connected to an upper end of the heat exchange jacket, a third cut-off valve is provided on the cold medium feed pipe, and a fourth cut-off valve is provided on the cold medium discharge pipe.
9. The carbazole refining system according to claim 8, wherein a heat medium feeding pipe is further connected to a lower end of the heat exchange jacket, a heat medium discharging pipe is further connected to an upper end of the heat exchange jacket, a fifth cut-off valve is provided on the heat medium feeding pipe, and a sixth cut-off valve is provided on the heat medium discharging pipe.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122223873.7U CN215781608U (en) | 2021-09-14 | 2021-09-14 | Carbazole system of refining |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202122223873.7U CN215781608U (en) | 2021-09-14 | 2021-09-14 | Carbazole system of refining |
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| CN215781608U true CN215781608U (en) | 2022-02-11 |
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| CN202122223873.7U Active CN215781608U (en) | 2021-09-14 | 2021-09-14 | Carbazole system of refining |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114736152A (en) * | 2022-04-08 | 2022-07-12 | 宁夏西泰煤化工有限公司 | Fine carbazole production method and production system |
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2021
- 2021-09-14 CN CN202122223873.7U patent/CN215781608U/en active Active
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114736152A (en) * | 2022-04-08 | 2022-07-12 | 宁夏西泰煤化工有限公司 | Fine carbazole production method and production system |
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