CN204454953U - A kind of circulation device for the production of nigrosine - Google Patents

A kind of circulation device for the production of nigrosine Download PDF

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Publication number
CN204454953U
CN204454953U CN201520021572.8U CN201520021572U CN204454953U CN 204454953 U CN204454953 U CN 204454953U CN 201520021572 U CN201520021572 U CN 201520021572U CN 204454953 U CN204454953 U CN 204454953U
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China
Prior art keywords
condenser
rectifying tower
aniline
water
lithium bromide
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CN201520021572.8U
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陈安源
王守满
刘方先
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QINGDAO DOUBLE-PEACH SPECIALITY CHEMICALS GROUP Co Ltd
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QINGDAO DOUBLE-PEACH SPECIALITY CHEMICALS GROUP Co Ltd
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    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02ATECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
    • Y02A30/00Adapting or protecting infrastructure or their operation
    • Y02A30/27Relating to heating, ventilation or air conditioning [HVAC] technologies
    • Y02A30/274Relating to heating, ventilation or air conditioning [HVAC] technologies using waste energy, e.g. from internal combustion engine
    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02BCLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
    • Y02B30/00Energy efficient heating, ventilation or air conditioning [HVAC]
    • Y02B30/62Absorption based systems
    • Y02B30/625Absorption based systems combined with heat or power generation [CHP], e.g. trigeneration

Abstract

The utility model relates to a kind of circulation device for the production of nigrosine, comprises condensation reaction still, acidification reaction still, rectifying tower, condenser and decker, wherein, is connected with whizzer between described acidification reaction still and rectifying tower; Be connected with lithium bromide chiller condenser between described rectifying tower and described condenser, described lithium bromide chiller condenser is provided with recirculated water entrance and circulating water outlet.The utility model effectively utilizes the aniline steam of rectifying tower top and the gas-phase potential heat of water vapor, low-pressure steam is utilized to drive lithium bromide chiller condenser, produce 7 DEG C of water to freeze for each workshop, 12 DEG C of water are converted into after each workshop reacting kettle jacketing or interchanger heat exchange, produce 7 DEG C of water cycles after entering lithium bromide chiller condenser condenses again to use, the heat of rectifying tower tower top is comprehensively effectively utilized, and economic benefit is obvious.Meanwhile, the raw material that the aniline of recovery can be used as nigrosine returns production technique recycle.

Description

A kind of circulation device for the production of nigrosine
Technical field
The utility model relates to technical field of dye, specifically, relates to a kind of circulation device for the production of nigrosine.
Background technology
Nigrosine is a kind of chemistry dyestuff, and its strong coloring force, dispersiveness is low, light absorptive good, color steadiness is high, and therefore to can be used for Plastic Resin painted for nigrosine, ink colorant, wood decoration technique is painted, leather, cotton, fiber crops dyeing and cover with paint, lacquer, colour wash, etc., the fields such as the painted and pigment coloration of metal products.
The waste water containing aniline can be produced in nigrosine production process, if directly discharge is very large to environmental hazard, but also can the wasting of resources be caused.Extract in aniline process utilizing rectifying tower, rectifying tower top can produce aniline steam and the water vapour of uniform flow, in per hour, the aniline steam of even generation 5310kg per hour and water vapour, this part gas mixture phase component contains a large amount of gas-phase potential heats, and its top gaseous phase latent heat is calculated as follows:
Known: 100 DEG C of water vapor enthalpys are: 2677KJ/Kg; The enthalpy of 100 DEG C of water is: 417.5KJ/Kg; Aniline enthalpy of vaporization is: 487.335KJ/Kg.
The gas-phase potential heat of rectifying tower tower top generation per hour is:
The Q always latent+Q water of latent=Q aniline dives
Q water is dived=0.84 × 5310 × (2677-417.5)=10078274KJ
Q aniline is dived=0.16 × 6000 × 487.335=414040KJ
Q is latent=10078274+414040=10492314KJ always
I.e. overhead vapours phase transformation generation latent heat per hour 10492314KJ, amounts to 249.8 ten thousand kilocalories.
Visible, containing a large amount of gas-phase potential heats in the gas mixture phase component of the aniline steam that rectifying tower tower top produces and water vapour, needing to carry out cooling process could aniline recovery.Ordinary method utilizes circulating water cooling or atmospheric condenser cooling, as Fig. 1 discloses a kind of schematic flow sheet of aniline distillation recovery device, waste water in storage tank 1 is containing aniline about 4%, the tower top of rectifying tower 3 is sent into after feed preheater 2 preheating, live steam directly enters at the bottom of the tower of rectifying tower 3, carry out stripping to containing aniline waste water, waste water at the bottom of tower is discharged after reclaiming preheating by feed preheater 2, send biochemical processing process.Tower top high concentration aniline gas-vapor mix condenses to through condenser 4 decker 5 that about 40 DEG C enter aniline, water, and upper strata aqueous phase contains a small amount of aniline, and send storage tank 1 back to and circulate distillation to reclaim aniline wherein, lower floor's aniline can recycle mutually.So not only can waste a large amount of recirculated water, and this partial heat also can not get effective utilization, thus cause the waste of this partial heat, financial loss is larger.
The recovery of aniline " in the alcohol soluble nigrosine factory effluent " [Wang Shouheng, Deng. the recovery [J] of aniline in alcohol soluble nigrosine factory effluent, 2009, 30 (3): 48-50] have also been devised a kind of device of improvement, as shown in Figure 2, squeeze in line mixer containing the aniline waste water lift pump 11 that contains of about 4%, add caustic soda neutralization and be adjusted to certain pH value, the storage tank 1 entering neutralizer after removal iron trichloride is filtered through manganese sand filter 12, in storage tank 1 aniline water aniline water pump boosting and after the shell side of feed preheater 2 is preheating to 90 DEG C by overhead vapours, send into the charging of rectifying tower 3 tower top.From rectifying tower 3 tower top steam out and wastewater feed heat exchange, uncooled steam enters after air cooler 15 is cooled to 60 DEG C, be mixed into condenser 4 with the condensation liquid phase of feed preheater 2 to continue to be cooled to about 40 DEG C, material after process send the decker 5 of aniline, water, equally, upper strata aqueous phase is sent storage tank 1 back to and is circulated distillation to reclaim aniline wherein, and lower floor's aniline is as raw material recycle in reaction process.At the bottom of the tower of rectifying tower 3, waste water first delivers to flash tank 14, then utilizes saturated waste water in injector 13 pairs of flash tanks 14 to carry out vacuum flashing, to reclaim heat, discharges after reclaiming preheating again.But utilize air cooler condensation not make full use of the gas-phase potential heat of tower top aniline steam and water vapour, thus cause and waste a large amount of heats.
In view of this, special proposition the utility model.
Utility model content
The purpose of this utility model is to provide a kind of circulation device producing nigrosine, this device effectively utilizes the aniline steam on aniline distillation tower top and the gas-phase potential heat of water vapor, low-pressure steam is utilized to drive lithium bromide chiller condenser, produce cold water to freeze for other workshops, the heat of aniline distillation tower tower top is comprehensively effectively utilized, and economic benefit is obvious.
For realizing the purpose of this utility model, the utility model adopts following technical scheme:
For the production of a circulation device for nigrosine, comprise condensation reaction still, acidification reaction still, rectifying tower, condenser and decker, wherein, between described acidification reaction still and rectifying tower, be connected with whizzer; Be connected with lithium bromide chiller condenser between described rectifying tower and described condenser, described lithium bromide chiller condenser is provided with recirculated water entrance and circulating water outlet.
At present, containing a large amount of gas-phase potential heats in the gas mixture phase component of the aniline steam that rectifying tower tower top produces and water vapor, needing to carry out cooling process could aniline recovery.Ordinary method utilizes circulating water cooling or atmospheric condenser cooling, and so not only can waste a large amount of recirculated water, and this partial heat also can not get effective utilization, thus cause the waste of this partial heat, financial loss is larger.
The utility model arranges whizzer at described acidification reaction still with being connected between rectifying tower, Working environment can be made to be that fully-closed operates by open type operation adjustment, effectively prevent the volatilization of material, protect environment; Improve the operating environment of worker.Simultaneously, the utility model effectively utilizes the aniline steam of rectifying tower top and the gas-phase potential heat of water vapor, low-pressure steam is utilized to drive lithium bromide chiller condenser, produce 7 DEG C of water to freeze for each workshop, 12 DEG C of water are converted into after each workshop reacting kettle jacketing or interchanger heat exchange, produce 7 DEG C of water cycles after entering lithium bromide chiller condenser condenses again to use, the heat of rectifying tower tower top is comprehensively effectively utilized, and economic benefit is obvious.Meanwhile, the raw material that the aniline reclaimed after rectifying tower stripping, lithium bromide chiller condenser condenses, condenser condenses and decker layering containing aniline waste water can be used as nigrosine returns production technique recycle.
In order to improve condensation effect further, condenser described in the utility model comprises the first condenser and the second condenser, and the first described condenser and the second condenser are connected in turn between described lithium bromide chiller condenser and decker.
Further, described lithium bromide chiller condenser is provided with aniline steam entry and aniline water out; Described aniline steam entry is connected by the tower top of pipeline with described rectifying tower; Described aniline water out is connected with the first described condenser by pipeline.
Preferably, the upside of described rectifying tower is also connected with static mixer.
Further, one end of described static mixer is provided with alkali liquor inlet and contains aniline waste water entrance, and the other end is connected with the upside of described rectifying tower.
Initial pH value containing the mother liquor of aniline waste water is acid, aniline exists with the form of hydrochloride, by connecting in the upside of rectifying tower, a static mixer is set, mother liquor containing aniline waste water is mixed from entering static mixer containing aniline waste water entrance, in static mixer, add liquid caustic soda mixing by alkali liquor inlet to neutralize simultaneously, after neutralization, aniline is converted into aniline by the form of anilinechloride, thus is convenient to rectifying.
In the utility model, the downside of described rectifying tower is provided with steam-in and condensation-water drain.
The steam-in of live steam on the downside of rectifying tower directly enters, and carry out stripping to containing aniline waste water, the steam condensate produced after stripping heat exchange flows out from described condensation-water drain.
In the utility model, described lithium bromide chiller condenser, the first described condenser and the second condenser are connected with cooling water supply pipe and CWR respectively.
As a kind of preferred version of the present utility model, at the bottom of the tower of rectifying tower described in the utility model, be connected with interchanger.
Containing heat waste water out at the bottom of rectifying tower, if directly send sewage work to process, the waste of this part heat will be caused.The utility model connects and arranges an interchanger at the bottom of rectifying tower, and waste water at the bottom of such tower enters sewage work's process after collecting heat by interchanger heat exchange again, thus avoids the waste of waste water heat at the bottom of tower.
Adopt the circulation device economic benefit for the production of nigrosine provided by the utility model obvious, by rectifying tower top generation per hour 5310Kg low-pressure steam, replacing 0.6MPa steam driven lithium bromide chiller to produce 7 DEG C of cool water quantities is 500m 3/ h, supply workshop refrigeration needs.Steam expense per ton is by 200 yuan of calculating, and the whole year can steam saving expense about 7,650,000.
Compared with prior art, the utility model tool has the following advantages:
(1) circulation device for the production of nigrosine provided by the utility model effectively can process aniline black dyestuffs waste water, realize the resource utilization of pollutent and the cleaner production of nigrosine, the removal of aniline can reduce the murder by poisoning to biochemical wastewater treatment, provides premise for sewage farm realizes qualified discharge; Meanwhile, the raw material that the aniline of recovery can be used as nigrosine returns production technique recycle;
(2) circulation device for the production of nigrosine provided by the utility model effectively utilizes the aniline steam of rectifying tower top and the gas-phase potential heat of water vapour, low-pressure steam is utilized to drive lithium bromide chiller condenser, produce 7 DEG C of water to freeze for each workshop, 12 DEG C of water are converted into after each workshop reacting kettle jacketing or interchanger heat exchange, drive after lithium bromide chiller through low-pressure steam again and produce 7 DEG C of water cycles uses, the heat of rectifying tower tower top is comprehensively effectively utilized, and economic benefit is obvious.
Accompanying drawing explanation
Fig. 1 is the structural representation of the aniline distillation recovery device of prior art;
Fig. 2 is the structural representation of the aniline distillation recovery device that prior art is improved;
Fig. 3 is the circulation device schematic diagram for the production of nigrosine provided by the utility model;
Wherein, in accompanying drawing, each component names is as follows:
1---storage tank, 2---feed preheater, 3---rectifying tower, 4---condenser, 41---the first condenser, 42---the second condenser, 5---decker, 6---lithium bromide chiller condenser, 7---static mixer, 8---interchanger, 9---cooling water supply pipe, 10---CWR, 11---lift pump, 12---manganese sand filter, 13---injector, 14---flash tank, 15---air cooler, 16---condensation reaction still, 17---acidification reaction still, 18---whizzer.
Embodiment
Below in conjunction with accompanying drawing, the utility model is described in further detail.
Embodiment one
As shown in Figure 3, the present embodiment provides a kind of circulation device for the production of nigrosine, comprise condensation reaction still 16, acidification reaction still 17, rectifying tower 3, condenser 4 and decker 5, wherein, between described acidification reaction still 17 and rectifying tower 3, be connected with whizzer 18; Be connected with lithium bromide chiller condenser 6 between described rectifying tower 3 and described condenser 4, described lithium bromide chiller condenser 6 is provided with recirculated water entrance and circulating water outlet.
The utility model arranges whizzer 18 at described acidification reaction still 17 with being connected between rectifying tower 3, Working environment can be made to be that fully-closed operates by open type operation adjustment, effectively prevent the volatilization of material, protect environment; Improve the operating environment of worker.Simultaneously, the utility model effectively utilizes the aniline steam of rectifying tower 3 tower top and the gas-phase potential heat of water vapor, low-pressure steam is utilized to drive lithium bromide chiller condenser 6, produce 7 DEG C of water to freeze for each workshop, 12 DEG C of water are converted into after each workshop reacting kettle jacketing or interchanger heat exchange, produce 7 DEG C of water cycles after entering lithium bromide chiller condenser 6 condensation again to use, the heat of rectifying tower 3 tower top is comprehensively effectively utilized, and economic benefit is obvious.Meanwhile, the raw material that the aniline reclaimed after rectifying tower 3 stripping, lithium bromide chiller condenser 6 condensation, condenser 4 condensation and decker 5 layering containing aniline waste water can be used as nigrosine returns production technique recycle.
In order to improve condensation effect further, condenser 4 described in the utility model comprises the first condenser 41 and the second condenser 42, and the first described condenser 41 and the second condenser 42 are connected in turn between described lithium bromide chiller condenser 6 and decker 5.
Described lithium bromide chiller condenser 6 is provided with aniline steam entry and aniline water out; Described aniline steam entry is connected by the tower top of pipeline with described rectifying tower 3; Described aniline water out is connected with the first described condenser 41 by pipeline.
The upside of described rectifying tower 3 is connected with static mixer 7.
One end of described static mixer 7 is provided with alkali liquor inlet and containing aniline waste water entrance, the other end is connected with the upside of described rectifying tower 3.
Initial pH value containing the mother liquor of aniline waste water is acid, aniline exists with the form of hydrochloride, by connecting in the upside of rectifying tower 3, a static mixer 7 is set, the mother liquor containing aniline waste water is made to enter static mixer 7 from containing aniline waste water entrance, in static mixer 7, add liquid caustic soda mixing by alkali liquor inlet to neutralize simultaneously, after neutralization, aniline is converted into aniline by the form of anilinechloride, thus is convenient to rectifying.
The downside of described rectifying tower 3 is provided with steam-in and condensation-water drain.
The steam-in of live steam on the downside of rectifying tower 3 directly enters, and carry out stripping to containing aniline waste water, the steam condensate produced after stripping heat exchange flows out from described condensation-water drain.
Described lithium bromide chiller condenser 6, the first described condenser 41 and the second condenser 42 are connected with cooling water supply pipe 9 and CWR 10 respectively.
The working process of a kind of circulation device for the production of nigrosine that the present embodiment provides comprises the steps:
(1) catalyzer, oil of mirbane and aniline are put in condensation reaction still 16 carry out condensation reaction, obtain the nigrosine product containing excessive aniline;
(2) in acidification reaction still 17, hot water and 30% hydrochloric acid is added, joined in acidification reaction still 17 by the nigrosine product containing excessive aniline of step (1) gained and carry out acidification reaction, the product obtained obtains nigrosine product by whizzer 18 is centrifugal and contains aniline waste water;
(3) mix from entering static mixer 7 containing aniline waste water entrance and alkali liquor inlet respectively by pipeline containing aniline waste water and alkali lye, rectifying tower 3 tower top is sent into after mixing, the steam-in of steam on the downside of rectifying tower 3 directly enters simultaneously, stripping is carried out, the waste water decontaminated water factory and office reason produced at the bottom of rectifying tower 3 tower after stripping to containing aniline waste water;
(4) aniline that after stripping, rectifying tower 3 tower top produces and the gas phase mixture of water enter lithium bromide chiller condenser 6 condensation; 12 DEG C of recirculated waters simultaneously from other workshops enter lithium bromide chiller condenser 6 by recirculated water entrance, the gas-phase potential heat produced by the gas phase mixture of aniline and water drives lithium bromide chiller condenser 6 to form 7 DEG C of recirculated waters to flow out from circulating water outlet and freeze for other workshop, is converted into 12 DEG C of recirculated waters and enters lithium bromide chiller condenser 6 by recirculated water entrance again and recycle after each workshop reacting kettle jacketing or interchanger heat exchange;
(5) gas phase mixture through lithium bromide chiller condenser 6 condensation becomes liquid phase mixture, condensation is carried out successively by the first condenser 41 and the second condenser 42, enter decker 5 after condensation and carry out layering, upper strata aqueous phase contains a small amount of aniline, sends the operation that step (3) are carried out in static mixer 7 circulation by pipeline back to from containing aniline waste water entrance; Lower floor's aniline returns as the raw material of synthesis nigrosine the operation that step (1) is carried out in production technique circulation.
Embodiment two
The present embodiment is the further improvement to embodiment one, for reclaiming at the bottom of rectifying tower 3 tower the heat of waste water out, connecting and arranging an interchanger 8 at the bottom of the tower of described rectifying tower 3.Containing heat waste water out at the bottom of rectifying tower 3 tower, if directly send sewage work to process, the waste of this part heat will be caused.The utility model connects and arranges an interchanger 8 at the bottom of rectifying tower 3 tower, and waste water at the bottom of such tower enters sewage work's process after first collecting heat by interchanger 8 heat exchange again, thus avoids the waste of waste water heat at the bottom of tower.
Comparative example
Contrasted by the device of device of the present utility model and prior art, wherein old device is the device of Fig. 1, and the device of improvement is the device of Fig. 2.The results are shown in shown in following table 1:
The new and old device of table 1, prior art and the major economic indicators of device of the present utility model contrast
Device provided by the utility model effectively utilizes the aniline steam of rectifying tower top and the gas-phase potential heat of water vapour on the one hand, low-pressure steam is utilized to drive lithium bromide chiller condenser, produce 7 degree of cold water for other workshops each refrigeration, the water of 12 degree is converted into after each workshop reacting kettle jacketing or interchanger heat exchange, the water cycle of generation 7 degree after lithium bromide chiller is driven to use through low-pressure steam again, the heat of rectifying tower tower top is comprehensively effectively utilized, and economic benefit is obvious.By rectifying tower top generation per hour 5310Kg low-pressure steam, replacing 0.6MPa steam driven lithium bromide chiller to produce 7 DEG C of cool water quantities is 500m 3/ h, supply workshop refrigeration needs.Steam expense per ton is by 200 yuan of calculating, and the whole year can steam saving expense about 7,650,000.On the other hand, compare with the device of improvement with old device, adopt circulation device of the present utility model to greatly reduce the consumption of recirculated water.
As mentioned above, plan content given by reference to the accompanying drawings, can derive similar technical scheme.In every case be the content not departing from technical solutions of the utility model, any simple modification done above embodiment according to technical spirit of the present utility model, equivalent variations and modification, all still belong in the scope of technical solutions of the utility model.

Claims (8)

1. the circulation device for the production of nigrosine, comprise condensation reaction still (16), acidification reaction still (17), rectifying tower (3), condenser (4) and decker (5), it is characterized in that, between described acidification reaction still (17) and rectifying tower (3), be connected with whizzer (18); Be connected with lithium bromide chiller condenser (6) between described rectifying tower (3) and described condenser (4), described lithium bromide chiller condenser (6) is provided with recirculated water entrance and circulating water outlet.
2. circulation device according to claim 1, it is characterized in that, described condenser (4) comprises the first condenser (41) and the second condenser (42), and described the first condenser (41) and the second condenser (42) are connected in turn between described lithium bromide chiller condenser (6) and decker (5).
3. circulation device according to claim 2, is characterized in that, described lithium bromide chiller condenser (6) is provided with aniline steam entry and aniline water out; Described aniline steam entry is connected by the tower top of pipeline with described rectifying tower (3); Described aniline water out is connected with described the first condenser (41) by pipeline.
4. circulation device according to claim 3, is characterized in that, the upside of described rectifying tower (3) is connected with static mixer (7).
5. circulation device according to claim 4, is characterized in that, one end of described static mixer (7) is provided with alkali liquor inlet and containing aniline waste water entrance, the other end is connected with the upside of described rectifying tower (3).
6. circulation device according to claim 5, is characterized in that, the downside of described rectifying tower (3) is provided with steam-in and condensation-water drain.
7. circulation device according to claim 6, it is characterized in that, described lithium bromide chiller condenser (6), described the first condenser (41) and the second condenser (42) are connected with cooling water supply pipe (9) and CWR (10) respectively.
8. the circulation device according to claim 1-7 any one, is connected with interchanger (8) at the bottom of the tower of described rectifying tower (3).
CN201520021572.8U 2015-01-13 2015-01-13 A kind of circulation device for the production of nigrosine Active CN204454953U (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104610175A (en) * 2015-01-13 2015-05-13 青岛双桃精细化工(集团)有限公司 Circulating device for producing nigrosine

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104610175A (en) * 2015-01-13 2015-05-13 青岛双桃精细化工(集团)有限公司 Circulating device for producing nigrosine
CN104610175B (en) * 2015-01-13 2017-01-04 青岛双桃精细化工(集团)有限公司 A kind of circulating device for producing nigrosine

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