CN206635250U - The purifying plant of permanent violet RL production process chlorobenzene mother liquors - Google Patents

The purifying plant of permanent violet RL production process chlorobenzene mother liquors Download PDF

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Publication number
CN206635250U
CN206635250U CN201720149192.1U CN201720149192U CN206635250U CN 206635250 U CN206635250 U CN 206635250U CN 201720149192 U CN201720149192 U CN 201720149192U CN 206635250 U CN206635250 U CN 206635250U
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China
Prior art keywords
chlorobenzene
pans
pipeline
heating kettle
purifying plant
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Expired - Fee Related
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CN201720149192.1U
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Chinese (zh)
Inventor
张蒙
于春发
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DONGTAI NEW JINTAI CHEMICAL Co Ltd
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DONGTAI NEW JINTAI CHEMICAL Co Ltd
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Abstract

The utility model discloses the purifying plant of permanent violet RL production process chlorobenzene mother liquors, including just steaming system and distillation system, first steaming system includes the first steaming kettle being sequentially connected by pipeline, First Heat Exchanger, just steam and receive water distributing can and just steaming chlorobenzene tank, distillation system includes heating kettle, rectifying column, second heat exchanger, product pans and front-end volatiles pans, the top of heating kettle is provided with heating kettle inlet and heating kettle liquid outlet, just steam chlorobenzene tank and heating kettle inlet is connected through first material pump by pipeline, gas outlet and rectifying column inlet are respectively equipped with the top and bottom of rectifying column, rectifying column inlet is connected with heating kettle liquid outlet, gas outlet connects the second heat exchanger by pipeline.The utility model can improve organic efficiency, and reduce distillation time using simply, securely and reliably.

Description

The purifying plant of permanent violet RL production process chlorobenzene mother liquors
Technical field
It the utility model is related to the production technical field of permanent violet, and in particular to a kind of permanent violet RL production processes chlorobenzene is female The purifying plant of liquid.
Background technology
In the nitration reaction of production permanent violet, N- ethyl carbazoles obtain after being nitrified during chlorobenzene is as the system of solvent To 3- nitro-N- ethyl carbazoles and the mixture of chlorobenzene, mixture is washed by filtering, filter cake with pull open powder, water washing, diafiltration For liquid after precipitation, lower floor is water containing pull open powder, the mother liquor of chlorobenzene.At present, the method for traditional recovery chlorobenzene uses for mother liquor The direct-fired mode of vapor, in the presence of vapor, chlorobenzene, pull open powder, water form azeotropic, chlorobenzene entrainment dampening, draw The foam and a small amount of impurity for opening powder formation are distilled out, and pull open powder, chlorobenzene in mother liquor, water are forced to present after steaming Buff, pressure separation and mother liquor composition difference due to azeotropic distillation, cause chlorobenzene content fluctuate it is larger, and content compared with It is low, the purity of chlorobenzene is reclaimed generally 95 ~ 97%.
Solvent of the chlorobenzene as nitrification, has a great influence to nitration reaction, and the impurity of chlorobenzene entrainment can be secondary with nitric acid progress Reaction, the impurity of sticky tarry is formed, so as to the quality in road after influenceing.For the quality of permanent violet pigment, and avoid by The washed difficulty of 3- nitro-N- ethyl carbazoles caused by the chlorobenzene content that feeds intake is too low, the purity for improving recovery chlorobenzene just seem It is particularly important.
The content of the invention
To solve the deficiencies in the prior art, the purpose of this utility model is that providing one kind uses simply, securely and reliably, can Organic efficiency is improved, and reduces the purifying plant of the permanent violet RL production process chlorobenzene mother liquors of distillation time.
In order to realize above-mentioned target, the utility model adopts the following technical scheme that:
The purifying plant of permanent violet RL production process chlorobenzene mother liquors, including system and distillation system are just steamed, just steam system bag Include the first steaming kettle being sequentially connected by pipeline, First Heat Exchanger, just steaming receives water distributing can and just steaming chlorobenzene tank, distillation system include Heating kettle, rectifying column, the second heat exchanger, product pans and front-end volatiles pans, the top of heating kettle are provided with heating kettle feed liquor Mouth and heating kettle liquid outlet, just steam chlorobenzene tank and heating kettle inlet, the top of rectifying column are connected through first material pump by pipeline Gas outlet and rectifying column inlet are respectively equipped with bottom, side top is provided with reflux inlet, rectifying column inlet and heating kettle Liquid outlet is connected, and gas outlet connects the import of the second heat exchanger by pipeline, and the outlet of the second heat exchanger is distinguished by pipeline The bottom liquid outlet of connection product pans and front-end volatiles pans, product pans and front-end volatiles pans passes through pipeline respectively Connect reflux inlet.
Preferably, foregoing heating kettle is chuck heating kettle, including chuck and cylinder, and steam inlet pipe is connected with the top of chuck With cooling water inlet pipe, effectively heating kettle can be heated or cooled.
More preferably, the foregoing just bottom of steaming kettle and heating kettle is equipped with slag-drip opening, and slag-drip opening is connected by Residue extraction pipeline Slag case, the top side of slag case are sequentially connected sack cleaner and air-introduced machine by pipeline.
It is highly preferred that the bottom inside foregoing rectifying column is provided with netted demister, netted demister between gas outlet according to Secondary to be provided with underfilling, middle filler and upper strata filler, underfilling is the high stainless steel Pall ring fillers of 2m, and middle filler is ZT-2 type regular corrugation fillers high 3m, upper strata filler are wire packing.
It is further preferred that before-mentioned products pans connect buffering with the top side of front-end volatiles pans by pipeline Tank.
Preferably, the top side of foregoing surge tank connects vavuum pump by pipeline, and vavuum pump selects water-jetting type vacuum Pump.
Specifically, it is equipped with atmospheric valve at the top of before-mentioned products pans, front-end volatiles pans and surge tank.
Preferably, before-mentioned products pans and the connecting pipe of front-end volatiles pans and reflux inlet are respectively equipped with the second thing Expect pump and 3 material pump, phegma can be sent into heating kettle.
More preferably, foregoing First Heat Exchanger and the second heat exchanger select shell and tube condenser or plate-type condenser.
It is highly preferred that being equipped with valve on all connecting pipes, valve is choke valve.
It is of the present utility model to be beneficial in that:Purifying plant of the present utility model is used for permanent violet Nitration of Chloronitrobenzene mother liquor Recovery, using simple, safe and reliable, first just steaming moisture, essence flows back to receipts chlorobenzene again, can improve distillation efficiency, make distillation time compared with Short and energy consumption is relatively low;Because of the guarantee of rear road rectifying, the speed for causing just to steam is accelerated, and can improve overall distillation speed.
Brief description of the drawings
Fig. 1 is structural representation of the present utility model.
The implication of reference in figure:1st, kettle is just steamed, 2, First Heat Exchanger, 3, just steam and receive water distributing can, 4, just steam chlorobenzene Tank, 5, heating kettle, 6, rectifying column, the 7, second heat exchanger, 8, product pans, 9, front-end volatiles pans, 10, first material pump, 11st, gas outlet, 12, reflux inlet, 13, second material pump, 14,3 material pump, 15, steam inlet pipe, 16, cooling water inlet Pipe, 17, slag case, 18, surge tank, 19, vavuum pump, 20, atmospheric valve.
Embodiment
Make specific introduce to the utility model below in conjunction with the drawings and specific embodiments.
Referring to Fig. 1, the purifying plant of permanent violet RL production processes chlorobenzene mother liquor of the present utility model, including just steam system and Distillation system, first steaming system receive the and of water distributing can 3 including the first steaming kettle 1, First Heat Exchanger 2, first steam being sequentially connected by pipeline Just steam chlorobenzene tank 4.
Distillation system includes heating kettle 5, rectifying column 6, the second heat exchanger 7, product pans 8 and front-end volatiles pans 9, adds The top of hot kettle 5 is provided with heating kettle inlet and heating kettle liquid outlet.Chlorobenzene tank 4 is just steamed by pipeline through first material pump 10 to connect Connect heating kettle inlet.The top and bottom of rectifying column 6 are respectively equipped with gas outlet 11 and rectifying column inlet, and side top is provided with Reflux inlet 12.
Rectifying column inlet is connected with heating kettle liquid outlet, and gas outlet 11 connects entering for the second heat exchanger 7 by pipeline Mouthful, the outlet of the second heat exchanger 7 connects product pans 8 and front-end volatiles pans 9, the He of product pans 8 by pipeline respectively The bottom liquid outlet of front-end volatiles pans 9 passes through pipeline communication reflux inlet 12 respectively.Receive in product pans 8 and front-end volatiles Phegma can be sent into by tank 9 with being respectively equipped with second material pump 13 and 3 material pump 14 on the connecting pipe of reflux inlet 12 In heating kettle 5, by controlling suitable reflux ratio, the yield of chlorobenzene can be improved.Wherein, First Heat Exchanger 2 and second exchanges heat Device 7 selects shell and tube condenser or plate-type condenser.
Heating kettle 5 is chuck heating kettle, including chuck and cylinder, and steam inlet pipe 15 and cooling water are connected with the top of chuck Inlet tube 16, effectively heating kettle 5 can be heated or cooled.Slag-drip opening is equipped with the bottom for just steaming kettle 1 and heating kettle 5, Slag-drip opening connects slag case 17 by Residue extraction pipeline, the top side of slag case 17 by pipeline be sequentially connected sack cleaner and Air-introduced machine, can discharge the fine dusts gone out in slag case 17 with waste residue and waste gas, and sack cleaner can be removed in waste gas Dust, avoid polluting environment.Upper valve and lower valve are provided with outside the slag-drip opening for just steaming kettle 1, Residue extraction pipeline is in two valves Between be communicated with jet chimney, when opening the slag-drip opening for just steaming kettle 1, first close lower valve, only open upper valve, discharge first Steam in kettle, avoid steaminess from entering slag case 17, and increased its internal pressure, and treated steam emptying, and open lower valve, discharge Waste residue.
During mother liquor distills, light component has part to produce certain foam, in order to preferably control foam Generation, avoids rushing tower, flooding phenomenon, the bottom inside rectifying column 6 is provided with netted demister, netted demister to gas outlet 11 Between be sequentially provided with underfilling, middle filler and upper strata filler, wherein underfilling is the high stainless steel Pall ring fillers of 2m, Middle filler is the high ZT-2 type regular corrugation fillers of 3m, and upper strata filler is wire packing.
ZT-2 type regular corrugation fillers are developed on common corrugated regular filler and the excellent combination foundation of random packing A kind of Novel standardized packing of the high comprehensive performance gone out.Optimization of the ZT-2 type fillers in structure makes gas-liquid flow rood to excellent Change, mass-transfer efficiency improves;The raising of its specific surface area increased number of theoretical plate, and filler rigidity etc. is superior to commonly Filler.These performances are favorably improved the separative efficiency and treating capacity of rectifying column 6, ensure to realize and improve product quality, extracting rate And the requirement for the treatment of capacity.
Surge tank 18, surge tank 18 are connected by pipeline with the top side of front-end volatiles pans 9 in product pans 8 Top side pass through pipeline and connect vavuum pump 19, vavuum pump 19 is from water-jetting type vavuum pump 19.Surge tank 18 can be to production Product pans 8 and front-end volatiles pans 9 play good cushioning effect, prevent that the uncooled gas content into liquid is more and makes Into pressure inside the tank it is excessive the problem of.The top of product pans 8, front-end volatiles pans 9 and surge tank 18 is equipped with atmospheric valve 20, Securely and reliably.
Valve is equipped with all connecting pipes of purifying plant of the present utility model, valve is choke valve.
In order to preferably illustrate the utility model, its course of work is specifically described below:
The mother liquor of nitration reaction is pumped into after precipitation removes water and just steams kettle 1.Under atmospheric pressure state, the first kettle 1 that steams is warming up to 100 DEG C, mother liquor is distilled, distillation fraction, which enters just to steam, receives water distributing can 3, and distillation finishes, and opens first steam and receives water distributing can 3 Bottom valve, first chlorobenzene is put into and just steams chlorobenzene tank 4, the later stage discharges the water on upper strata;The chlorobenzene just steamed in chlorobenzene tank 4 passes through the first thing Material pump 10 is transferred in heating kettle 5, carries out rectifying, and front-end volatiles enter front-end volatiles collecting tank, then cools down kettle temperature to 60 DEG C, is opened true Empty set is united and the heating of the chuck of heating kettle 5, while controls the reflux ratio 2 of rectifying column 6:1, chlorobenzene in the presence of vacuum and reflux ratio, By steaming progressively, enter product pans 8 after the condensation of the second heat exchanger 7, distill to the lower section of the second heat exchanger 7 and regard cup base When this no liquid comes out, slagging, chuck cooling.
The utility model uses just distillation to chlorobenzene mother liquor first, can force quickly to steam by chlorobenzene, and remove wherein Moisture, recycle rectifying column device recovery chlorobenzene, reclaim the purity of chlorobenzene up to more than 99.3%, color is water white transparency; As a result of vacuum distillation in distillation process, distillation time is shorter and energy consumption is relatively low;Simultaneously as the guarantor of You Liaohou roads rectifying Card, cause the speed just steamed to accelerate, although the content just steamed is decreased slightly as low, improve overall distillation speed.
In description of the present utility model, it is to be understood that term " " center ", " longitudinal direction ", " transverse direction ", " on ", " under ", The orientation or position relationship of the instruction such as "front", "rear", "left", "right", " vertical ", " level ", " top ", " bottom ", " interior ", " outer " are Based on orientation shown in the drawings or position relationship, it is for only for ease of description the utility model and simplifies description, rather than instruction Or imply that signified device or element must have specific orientation, with specific azimuth configuration and operation, therefore be not understood that For to limitation of the present utility model.In addition, term " first ", " second " be only used for describe purpose, and it is not intended that instruction or Imply relative importance.
, it is necessary to which explanation, unless otherwise clearly defined and limited, term " are pacified in description of the present utility model Dress ", " connected ", " connection " should be interpreted broadly, for example, it may be fixedly connected or be detachably connected, or integratedly Connection;Can be mechanical connection or electrical connection;Can be joined directly together, can also be indirectly connected by intermediary, It can be the connection of two element internals.For the ordinary skill in the art, above-mentioned art can be understood with concrete condition Concrete meaning of the language in the utility model.
General principle, principal character and advantage of the present utility model has been shown and described above.The technical staff of the industry It should be appreciated that above-described embodiment does not limit the utility model in any form, it is all by the way of equivalent substitution or equivalent transformation The technical scheme obtained, all falls within the scope of protection of the utility model.

Claims (10)

1. the purifying plant of permanent violet RL production process chlorobenzene mother liquors, including just steam system and distillation system, it is characterised in that institute First steaming kettle, First Heat Exchanger, just steaming of the first steaming system including being sequentially connected by pipeline is stated to receive water distributing can and just steam chlorobenzene tank, The distillation system includes heating kettle, rectifying column, the second heat exchanger, product pans and front-end volatiles pans, the heating kettle Top be provided with heating kettle inlet and heating kettle liquid outlet, it is described just steam chlorobenzene tank by pipeline through the connection of first material pump plus Hot kettle inlet, gas outlet and rectifying column inlet is respectively equipped with the top and bottom of the rectifying column, side top is provided with back Inflow entrance, the rectifying column inlet are connected with heating kettle liquid outlet, and the gas outlet connects the second heat exchanger by pipeline Import, the outlet of second heat exchanger connects product pans and front-end volatiles pans, the product by pipeline respectively The bottom liquid outlet of pans and front-end volatiles pans passes through pipeline communication reflux inlet respectively.
2. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that described to add Hot kettle is chuck heating kettle, including chuck and cylinder, and steam inlet pipe and cooling water inlet pipe are connected with the top of the chuck.
3. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that described first The bottom for steaming kettle and heating kettle is equipped with slag-drip opening, and the slag-drip opening connects slag case by Residue extraction pipeline, the slag case Top side is sequentially connected sack cleaner and air-introduced machine by pipeline.
4. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that the essence Evaporate the bottom inside tower and be provided with netted demister, netted demister is to being sequentially provided with underfilling, middle filler between gas outlet With upper strata filler, the underfilling is the high stainless steel Pall ring fillers of 2m, and the middle filler is the high ZT-2 types rule of 3m Whole ripple packing, the upper strata filler are wire packing.
5. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that the production Product pans connect surge tank with the top side of front-end volatiles pans by pipeline.
6. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 5, it is characterised in that described slow The top side for rushing tank connects vavuum pump by pipeline, and the vavuum pump selects water-jetting type vavuum pump.
7. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 5, it is characterised in that the production Atmospheric valve is equipped with the top of product pans, front-end volatiles pans and surge tank.
8. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that the production Second material pump and 3 material pump are respectively equipped with product pans and the connecting pipe of front-end volatiles pans and reflux inlet.
9. the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to claim 1, it is characterised in that described One heat exchanger and the second heat exchanger select shell and tube condenser or plate-type condenser.
10. according to the purifying plant of permanent violet RL production processes chlorobenzene mother liquor according to any one of claims 1 to 9, it is special Sign is, valve is equipped with all connecting pipes, and the valve is choke valve.
CN201720149192.1U 2017-02-20 2017-02-20 The purifying plant of permanent violet RL production process chlorobenzene mother liquors Expired - Fee Related CN206635250U (en)

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CN201720149192.1U CN206635250U (en) 2017-02-20 2017-02-20 The purifying plant of permanent violet RL production process chlorobenzene mother liquors

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Application Number Priority Date Filing Date Title
CN201720149192.1U CN206635250U (en) 2017-02-20 2017-02-20 The purifying plant of permanent violet RL production process chlorobenzene mother liquors

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848338A (en) * 2020-08-27 2020-10-30 银川百泓新材料科技有限公司 Method and device for recovering o-dichlorobenzene from permanent violet centrifugal mother liquor

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111848338A (en) * 2020-08-27 2020-10-30 银川百泓新材料科技有限公司 Method and device for recovering o-dichlorobenzene from permanent violet centrifugal mother liquor
CN111848338B (en) * 2020-08-27 2023-12-22 银川百泓新材料科技有限公司 Method and device for recovering o-dichlorobenzene from permanent violet centrifugal mother liquor

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Granted publication date: 20171114

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