CN213060225U - System for retrieve sodium bromide in follow carbazole alkylation waste lye - Google Patents
System for retrieve sodium bromide in follow carbazole alkylation waste lye Download PDFInfo
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- CN213060225U CN213060225U CN202021866730.7U CN202021866730U CN213060225U CN 213060225 U CN213060225 U CN 213060225U CN 202021866730 U CN202021866730 U CN 202021866730U CN 213060225 U CN213060225 U CN 213060225U
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Abstract
The utility model provides a system for retrieve sodium bromide from carbazole alkylation waste lye belongs to permanent purple production technical field. The method is characterized in that an alkaline water collecting pool, an evaporation concentration device, a cooling crystallization device and a sodium bromide suction filtration device are sequentially arranged, alkaline water separated from the bottom layer of an alkylation reaction kettle is firstly sent into the alkaline water collecting pool to be accumulated, then is sent into the evaporation concentration device by a pump to be evaporated and concentrated, concentrated solution is discharged into the cooling crystallization device to be cooled, and sodium bromide is crystallized and separated out. And feeding the slurry containing sodium bromide into a sodium bromide suction filtration device, carrying out suction filtration and separation to obtain filtrate and filter cakes, recycling the filtrate as liquid caustic soda, and packaging and selling the filter cakes as industrial sodium bromide. The system treats the waste alkali liquor generated in the carbazole alkylation process to obtain the waste water, the liquid alkali and the sodium bromide product with low salt content, so that the sodium bromide and the sodium hydroxide in the carbazole alkylation waste alkali liquor are recycled, and the difficulty in wastewater treatment is reduced.
Description
Technical Field
The utility model belongs to the technical field of the permanent violet production, concretely relates to retrieve system of sodium bromide from carbazole alkylation waste lye.
Background
The permanent violet RL is a high-grade organic pigment of dioxazine class, has outstanding tinting strength and brightness, excellent heat resistance and penetration resistance and good light fastness, has wide application range, and is popular in the fields of paint, plastics, organic glass, rubber, textile printing, solvent ink, water-based ink, packaging printing and the like.
The permanent violet RL is produced by the following main processes: dissolving carbazole in alkali solution for alkylation to obtain N-ethyl carbazole, nitrating N-ethyl carbazole in nitric acid, and then H2Reducing, condensing in tetrachlorobenzoquinone, ring-closing in benzene sulfonyl chloride, oxidizing to obtain crude permanent violet liquid, filtering, drying, crushing and other steps. The method mainly comprises the steps of adding carbazole and a catalyst into prepared liquid alkali, heating to 60-90 ℃, refluxing and dropwise adding bromoethane for 2-5 h, and reacting for 2-5 h under heat preservation. Sampling to detect that the content of carbazole is less than or equal to 0.5, distilling to 120-140%And (4) layering the lower layer of alkaline water into an alkaline water pool.
Through detection and analysis, the alkaline water generated in the carbazole alkylation process mainly contains sodium bromide, sodium hydroxide and a small amount of organic components, and generally, the part of alkaline water is used as neutralization alkali in wastewater treatment or directly used as wastewater to be discharged, so that the sodium bromide and the sodium hydroxide in the wastewater are wasted, the salt content of the wastewater is too high, and the wastewater treatment difficulty and the wastewater treatment cost are increased.
Disclosure of Invention
In view of this, the utility model provides a system for retrieve sodium bromide from carbazole alkylation waste lye to solve the wasting of resources that the direct emission of carbazole alkylation waste water that exists among the prior art leads to, the technical problem that the waste water treatment degree of difficulty improves.
The utility model provides a technical scheme that its technical problem adopted is:
a system for recovering sodium bromide from carbazole alkylation spent caustic, comprising:
the alkaline water collecting pool is used for collecting waste alkaline liquid generated in the carbazole alkylation process;
the feed end of the evaporation concentration device is connected with the alkaline water collecting tank and is used for concentrating the waste alkaline liquid from the alkaline water collecting tank;
the feed end of the cooling crystallization device is connected with the discharge end of the evaporation concentration device and is used for cooling the concentrated solution of the waste alkali liquor and separating out sodium bromide; and
and the feed end of the sodium bromide suction filtration device is connected with the discharge end of the cooling crystallization device and is used for obtaining a sodium bromide filter cake through suction filtration.
Preferably, the evaporation concentration device comprises an evaporation concentration tower, a wastewater collection assembly is arranged on the top of the evaporation concentration tower, a heating assembly is arranged at the tower bottom, the wastewater collection assembly comprises a condenser, a condensate tank and a reflux discharge pump which are sequentially connected, and the heating assembly comprises a tower bottom circulating pump and a tower bottom reboiler which are sequentially connected.
Preferably, a vacuum pump is further arranged on the evaporation concentration tower.
Preferably, a concentration liquid level meter is arranged on the evaporation concentration tower.
Preferably, the cooling crystallization device is a centrifuge.
Preferably, a cooling jacket is arranged on the outer side of the cooling crystallization device, and a circulating water upper water pipe and a circulating water return pipe are connected to the cooling jacket.
Preferably, a temperature controller is arranged on the cooling crystallization device, a circulating water control valve is arranged on the circulating water upper water pipe, and the circulating water control valve is electrically connected with the temperature controller.
Preferably, the centrifugal mother liquid discharge end of the cooling crystallization device is connected with a liquid caustic soda recovery tank.
Preferably, the filtrate discharge end of the sodium bromide suction filtration device is connected with the liquid caustic soda recovery tank.
According to the above technical scheme, the utility model provides a retrieve system of sodium bromide in follow carbazole alkylation waste lye, its beneficial effect is: the device is characterized in that the alkaline water collecting pool, the evaporation concentration device, the cooling crystallization device and the sodium bromide suction filtration device are sequentially arranged, and alkaline water separated from the bottom layer of the alkylation reaction kettle is firstly fed into the alkaline water collecting pool to be accumulated in the carbazole alkylation process. The alkaline water in the alkaline water collecting pool is firstly pumped into the evaporation concentration device for evaporation concentration, water is condensed and collected, and concentrated solution is discharged into the cooling crystallization device for cooling, so that sodium bromide is crystallized and separated out. And feeding the slurry containing the sodium bromide into the sodium bromide suction filtration device, carrying out suction filtration and separation to obtain filtrate and filter cakes, recycling the filtrate as liquid caustic soda, and packaging and selling the filter cakes as industrial sodium bromide. The system for recovering the sodium bromide from the carbazole alkylation waste alkali liquor treats the waste alkali liquor generated in the carbazole alkylation process to obtain the wastewater, the liquid alkali and the sodium bromide product with low salt content, so that the sodium bromide and the sodium hydroxide in the carbazole alkylation waste alkali liquor are recycled, the wastewater treatment difficulty is reduced, and the wastewater treatment cost is reduced.
Drawings
FIG. 1 is a schematic flow diagram of a system for recovering sodium bromide from carbazole alkylation spent lye.
In the figure: the system comprises a system 10 for recovering sodium bromide from carbazole alkylation waste alkali liquor, an alkali water collecting pool 100, an alkali water discharge pump 110, an evaporation concentration device 200, a condenser 211, a condensate tank 212, a reflux discharge pump 213, a tower kettle circulating pump 221, a tower kettle reboiler 222, a vacuum pump 230, a concentration liquid level meter 240, a cooling crystallization device 300, a cooling jacket 310, a circulating water upper water pipe 311, a circulating water return pipe 312, a circulating water control valve 313, a temperature controller 320, a liquid alkali recovery tank 330 and a sodium bromide suction filtration device 400.
Detailed Description
The following combines the drawings of the utility model to further elaborate the technical scheme and technical effect of the utility model.
Referring to FIG. 1, in one embodiment, a system 10 for recovering sodium bromide from carbazole alkylation spent caustic is used for treating the spent caustic generated during carbazole alkylation and recycling sodium bromide components in the spent caustic. The method comprises the following steps: the device comprises an alkaline water collecting tank 100, an evaporation concentration device 200, a cooling crystallization device 300 and a sodium bromide suction filtration device 400.
The alkaline water collecting tank 100 is connected to the bottom of the carbazole alkylation reaction kettle and is used for collecting waste alkaline liquid generated in the carbazole alkylation process. An alkaline water discharge pump 110 is arranged on the alkaline water collecting tank 100 and used for discharging the alkaline water collected in the alkaline water collecting tank 100.
The feed end of the evaporation concentration device 200 is connected to the alkaline water collection tank 100, that is, the feed end of the evaporation concentration device 200 is connected to the outlet end of the alkaline water discharge pump 110, and is used for concentrating the waste alkaline water from the alkaline water collection tank 100. For example, the evaporation concentration device 200 includes an evaporation concentration tower, a wastewater collection component is disposed on the top of the evaporation concentration tower, a heating component is disposed on the bottom of the evaporation concentration tower, the wastewater collection component includes a condenser 211, a condensate tank 212 and a reflux discharge pump 213, which are connected in sequence, and the heating component includes a bottom circulation pump 221 and a bottom reboiler 222, which are connected in sequence. The evaporation concentration tower receives alkaline water pumped by the alkaline water discharge pump 110, the alkaline water is forced to circulate under the action of the tower kettle circulating pump 221, and is heated by the tower kettle reboiler 222 until the tower kettle temperature of the evaporation concentration tower is 80-95 ℃, water in the alkaline water is gasified, and the alkaline water is discharged from the top of the evaporation concentration tower. The gasified water is condensed by the condenser 211, the condensate is collected in the condensate tank 212, and the reflux discharge pump 213 refluxes a part of the condensate collected in the condensate tank 212 and discharges a part of the condensate as wastewater. After the salt content in the concentrated solution in the tower bottom of the evaporation concentration tower reaches a predetermined concentration, the concentrated solution is conveyed to the cooling crystallization device 300 through the tower bottom circulating pump 221.
In a preferred embodiment, the evaporation concentration tower is further provided with a vacuum pump 230 to provide negative pressure for the evaporation concentration device 200 system, so as to implement reduced pressure distillation and reduce the temperature of the bottom of the evaporation concentration tower, thereby reducing energy consumption and improving evaporation concentration efficiency.
In another preferred embodiment, the evaporation concentration tower is provided with a concentration liquid level meter 240, so that during evaporation concentration, the concentration degree of the alkaline water is judged by the liquid level drop of the concentration liquid level meter 240, and the phenomenon that the concentration degree is too high, sodium bromide is separated out in advance or sodium hydroxide is separated out together, and the concentration degree is too low, so that sodium bromide cannot reach saturation and cannot be separated out is avoided.
The feed end of the cooling crystallization device 300 is connected with the discharge end of the evaporation concentration device 200, namely, the feed end of the cooling crystallization device 300 is connected with the outlet end of the tower kettle circulating pump 221, and is used for cooling the concentrated solution of the waste alkali liquor and separating out sodium bromide. For example, the cooling crystallization device 300 is a centrifuge, a cooling jacket 310 is disposed outside the centrifuge, and a circulating water inlet pipe 311 and a circulating water return pipe 312 are connected to the cooling jacket 310. The concentrated solution at the bottom of the evaporation concentration kettle is discharged into the cooling crystallization device 300, at the moment, sodium bromide is not separated out at high temperature, circulating water is introduced into the cooling jacket 310 through the circulating water upper water pipe 311 and the circulating water return pipe 312, the concentrated solution in the cooling crystallization device 300 is cooled, sodium bromide is separated out along with the temperature reduction, and liquid caustic soda and sodium bromide are centrifugally separated at low temperature.
Further, in order to control the cooling temperature and prevent sodium hydroxide precipitation caused by too low temperature, the cooling crystallization device 300 is provided with a temperature controller 320, the circulating water feeding pipe 311 is provided with a circulating water control valve 313, and the circulating water control valve 313 is electrically connected with the temperature controller 320. That is, the temperature of the concentrated solution in the cooling crystallization device 300 is automatically adjusted by the circulating water amount control valve 313 and the temperature controller 320, so that the sodium bromide is precipitated to the maximum amount and the sodium hydroxide is not precipitated.
In an embodiment, a centrifugal mother liquid discharge end of the cooling crystallization device 300 is connected to a liquid caustic recovery tank 330 to recycle liquid caustic centrifugally separated in the cooling crystallization device 300.
And the feed end of the sodium bromide suction filtration device 400 is connected with the discharge end of the cooling crystallization device 300 and is used for obtaining a sodium bromide filter cake through suction filtration. The sodium bromide suction filtration device 400 further dehydrates sodium bromide from the cooling crystallization device 300, reduces the content of the sodium bromide, and obtains industrial sodium bromide.
In an embodiment, a filtrate discharge end of the sodium bromide suction filtration device 400 is connected to the liquid caustic soda recovery tank 330, so as to recycle the liquid caustic soda separated in the sodium bromide suction filtration device 400.
The system 10 for recovering sodium bromide from carbazole alkylation waste alkali liquid treats the waste alkali liquid generated in the carbazole alkylation process to obtain wastewater, liquid alkali and sodium bromide products with low salt content, so that sodium bromide and sodium hydroxide in the carbazole alkylation waste alkali liquid are recycled, the wastewater treatment difficulty is reduced, and the wastewater treatment cost is reduced.
While the invention has been described with reference to a preferred embodiment, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention.
Claims (9)
1. A system for recovering sodium bromide from carbazole alkylation waste lye is characterized by comprising:
the alkaline water collecting pool is used for collecting waste alkaline liquid generated in the carbazole alkylation process;
the feed end of the evaporation concentration device is connected with the alkaline water collecting tank and is used for concentrating the waste alkaline liquid from the alkaline water collecting tank;
the feed end of the cooling crystallization device is connected with the discharge end of the evaporation concentration device and is used for cooling the concentrated solution of the waste alkali liquor and separating out sodium bromide; and
and the feed end of the sodium bromide suction filtration device is connected with the discharge end of the cooling crystallization device and is used for obtaining a sodium bromide filter cake through suction filtration.
2. The system for recovering sodium bromide from carbazole alkylation spent lye according to claim 1, wherein the evaporation concentration device comprises an evaporation concentration tower, the top of the evaporation concentration tower is provided with a waste water collection assembly, the bottom of the tower is provided with a heating assembly, the waste water collection assembly comprises a condenser, a condensate tank and a reflux discharge pump which are connected in sequence, and the heating assembly comprises a bottom circulating pump and a bottom reboiler which are connected in sequence.
3. The system for recovering sodium bromide from carbazole-alkylated spent caustic according to claim 2, wherein a vacuum pump is further provided on the evaporation concentration tower.
4. The system for recovering sodium bromide from carbazole-alkylated spent caustic according to claim 2, wherein a concentration level gauge is disposed on the evaporation concentration tower.
5. The system for recovering sodium bromide from carbazole alkylation spent caustic according to claim 1, wherein the temperature-reducing crystallization device is a centrifuge.
6. The system for recovering sodium bromide from carbazole alkylation spent lye according to claim 5, wherein a cooling jacket is arranged outside the cooling crystallization device, and the cooling jacket is connected with a circulating water upper water pipe and a circulating water return pipe.
7. The system for recovering sodium bromide from carbazole alkylation spent lye according to claim 6, wherein a temperature controller is arranged on the cooling crystallization device, a circulating water control valve is arranged on the circulating water upper pipe, and the circulating water control valve is electrically connected with the temperature controller.
8. The system for recovering sodium bromide from carbazole alkylation spent lye according to claim 5, wherein the centrifugal mother liquor discharge end of the cooling crystallization device is connected with a liquid caustic recovery tank.
9. The system for recovering sodium bromide from carbazole alkylation spent lye according to claim 8, wherein the filtrate discharge end of the sodium bromide suction filtration device is connected with the liquid caustic recovery tank.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021866730.7U CN213060225U (en) | 2020-08-31 | 2020-08-31 | System for retrieve sodium bromide in follow carbazole alkylation waste lye |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202021866730.7U CN213060225U (en) | 2020-08-31 | 2020-08-31 | System for retrieve sodium bromide in follow carbazole alkylation waste lye |
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| Publication Number | Publication Date |
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| CN213060225U true CN213060225U (en) | 2021-04-27 |
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| CN202021866730.7U Active CN213060225U (en) | 2020-08-31 | 2020-08-31 | System for retrieve sodium bromide in follow carbazole alkylation waste lye |
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