CN104610175B - A kind of circulating device for producing nigrosine - Google Patents
A kind of circulating device for producing nigrosine Download PDFInfo
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- CN104610175B CN104610175B CN201510016605.4A CN201510016605A CN104610175B CN 104610175 B CN104610175 B CN 104610175B CN 201510016605 A CN201510016605 A CN 201510016605A CN 104610175 B CN104610175 B CN 104610175B
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A30/00—Adapting or protecting infrastructure or their operation
- Y02A30/27—Relating to heating, ventilation or air conditioning [HVAC] technologies
- Y02A30/274—Relating to heating, ventilation or air conditioning [HVAC] technologies using waste energy, e.g. from internal combustion engine
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- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
- Y02B30/00—Energy efficient heating, ventilation or air conditioning [HVAC]
- Y02B30/62—Absorption based systems
- Y02B30/625—Absorption based systems combined with heat or power generation [CHP], e.g. trigeneration
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Abstract
The present invention relates to a kind of circulating device for producing nigrosine, including condensation reaction still, acidification reaction still, rectifying column, condenser and decker, wherein, between described acidification reaction still and rectifying column, be connected with centrifuge；Being connected with lithium bromide chiller condenser between described rectifying column and described condenser, described lithium bromide chiller condenser is provided with recirculated water entrance and circulating water outlet.The present invention effectively utilizes aniline steam and the gas-phase potential heat of water vapour of rectifying tower top, 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 it are converted into after each workshop reacting kettle jacketing or heat exchanger heat exchange, produce 7 DEG C of water after entering back into the condensation of lithium bromide chiller condenser to recycle, the heat making rectifying column tower top is comprehensively effectively utilized, and economic benefit is obvious.Meanwhile, the aniline of recovery can recycle as the raw material return production technology of nigrosine.
Description
Technical field
The present invention relates to technical field of dye, specifically, relate to a kind of circulating device for producing nigrosine.
Background technology
Nigrosine is a kind of chemistry dyestuff, and its strong coloring force, dispersibility are low, light absorptive good, color steadiness high, therefore
Nigrosine can be used for plastic resin coloring, ink colorant, and wood decoration technique colours, leather, cotton, fiber crops dyeing and covering with paint, metal
The field such as color articles and pigment coloration.
The waste water containing aniline can be produced in nigrosine production process, if directly discharge is very big to environmental hazard,
But also the wasting of resources can be caused.During utilizing rectifying column to extract aniline, rectifying column top can produce the benzene of uniform flow
Amine steam and steam, in terms of per hour, the most uniformly produce aniline steam and the steam of 5310kg, this part gaseous mixture
Phase component contains substantial amounts of gas-phase potential heat, and its top gaseous phase latent heat is calculated as follows:
Known: 100 DEG C of water vapour 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 that rectifying column tower top produces per hour is:
Latent+Q the water of Q always latent=Q aniline is dived
Q water is dived=0.84 × 5310 × (2677-417.5)=10078274KJ
Q aniline is dived=0.16 × 6000 × 487.335=414040KJ
Q always latent=10078274+414040=10492314KJ
I.e. overhead vapours phase transformation produces latent heat 10492314KJ per hour, equivalent 249.8 ten thousand kilocalories.
Visible, the aniline steam of rectifying column tower top generation and the gaseous mixture phase component of steam are dived containing substantial amounts of gas phase
Heat, needs to carry out cooling and processes ability aniline recovery.Conventional method is to utilize circulating water cooling or aerial condenser cooling, as
Fig. 1 discloses the schematic flow sheet of a kind of aniline distillation recovery device, and the waste water in storage tank 1 contains aniline about 4%, pre-through charging
Sending into the tower top of rectifying column 3 after the preheating of hot device 2, live steam is directly entered from the bottom of the tower of rectifying column 3, carries out containing aniline waste water
Stripping, waste water at the bottom of tower is discharged after reclaiming preheating by feed preheater 2, is sent biochemical processing process.Tower top high concentration aniline steam
The condensed device of mixture 4 condenses to about 40 DEG C and enters aniline, the decker 5 of water, and upper strata aqueous phase contains a small amount of aniline, sends back to
Storage tank 1 circulation distillation is to reclaim aniline therein, and lower floor's aniline can recycle mutually.The most not only can waste substantial amounts of circulation
Water, and this partial heat also can not get effectively utilizing, thus cause the waste of this partial heat, economic loss is bigger.
" recovery of alcohol soluble nigrosine production Aniline " [Wang Shouheng, etc. alcohol soluble nigrosine produces Aniline
Reclaim [J], 2009,30 (3): 48-50] have also been devised the device of a kind of improvement, as in figure 2 it is shown, containing about 4% give up containing aniline
Water elevator pump 11 is squeezed in pipe-line mixer, adds in Caustic soda and regulation is to certain pH value, filter through manganese sand filter 12 and remove
Entering the storage tank 1 of neutralizer after ferric chloride, the aniline water in storage tank 1 is with the boosting of aniline water pump and at the shell of feed preheater 2
After journey is preheating to 90 DEG C by overhead vapours, send into the charging of rectifying column 3 tower top.Enter with waste water from rectifying column 3 tower top steam out
Material heat exchange, after uncooled steam entrance air cooler 15 is cooled to 60 DEG C, is mixed into cold with the condensation liquid phase of feed preheater 2
Condenser 4 continues to be cooled to about 40 DEG C, and the material after process send the decker 5 of aniline, water, and equally, upper strata aqueous phase sends storage back to
Tank 1 circulation distillation is to reclaim aniline therein, and lower floor's aniline recycles in reaction process as raw material.Rectifying column 3
Waste water at the bottom of tower first delivers to flash tank 14, then utilizes ejector 13 that waste water saturated in flash tank 14 is carried out vacuum flashing, to return
Receive heat, discharge again after reclaiming preheating.But utilize air cooler condensation not make full use of tower top aniline steam
With the gas-phase potential heat of steam, thus cause and waste substantial amounts of heat.
In view of this, the special proposition present invention.
Summary of the invention
It is an object of the invention to provide a kind of circulating device producing nigrosine, this device effectively utilizes aniline distillation tower
The aniline steam on top and the gas-phase potential heat of water vapour, utilize low-pressure steam to drive lithium bromide chiller condenser, produces cold water for it
He uses workshop refrigeration, makes the heat of aniline distillation tower tower top comprehensively be effectively utilized, and economic benefit is obvious.
For realizing the purpose of the present invention, the present invention adopts the following technical scheme that
A kind of circulating device for producing nigrosine, including condensation reaction still, acidification reaction still, rectifying column, condenser
And decker, wherein, between described acidification reaction still and rectifying column, it is connected with centrifuge；Described rectifying column is with described
Condenser between be connected with lithium bromide chiller condenser, described lithium bromide chiller condenser be provided with recirculated water entrance and
Circulating water outlet.
At present, the aniline steam of rectifying column tower top generation and the gaseous mixture phase component of water vapour are dived containing substantial amounts of gas phase
Heat, needs to carry out cooling and processes ability aniline recovery.Conventional method is to utilize circulating water cooling or aerial condenser cooling, this
Sample not only can waste substantial amounts of recirculated water, and this partial heat also can not get effectively utilizing, thus causes this partial heat
Waste, economic loss is bigger.
The present invention is connected between described acidification reaction still and rectifying column and arranges centrifuge, and working environment can be made by opening wide
Formula operation adjustment is total enclosing operation, effectively prevents the volatilization of material, protects environment；Improve the operating environment of worker.With
Time, the present invention effectively utilizes aniline steam and the gas-phase potential heat of water vapour of rectifying tower top, utilizes low-pressure steam to drive lithium bromide
Train condenser, produces 7 DEG C of water and freezes for each workshop, converts after each workshop reacting kettle jacketing or heat exchanger heat exchange
It is 12 DEG C of water, produces 7 DEG C of water after entering back into the condensation of lithium bromide chiller condenser and recycle, make the heat of rectifying column tower top obtain
Comprehensively effectively utilizing, economic benefit is obvious.Meanwhile, containing aniline waste water through rectifying column stripping, lithium bromide chiller condenser condensation,
The aniline that condenser condensation and decker reclaim after being layered can return production technology as the raw material of nigrosine and recycle.
In order to improve condensation effect further, condenser of the present invention includes the first condenser and the second condenser,
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 be connected by the tower top of pipeline with described rectifying column；Described aniline water out by pipeline with
The first described condenser is connected.
Preferably, the upside of described rectifying column is also connected with being provided with static mixer.
Further, one end of described static mixer is provided with alkali liquor inlet and the entrance Han aniline waste water, the other end with
The upside of described rectifying column is connected.
The original ph of the mother solution containing aniline waste water is acid, and aniline is presented in hydrochlorate, by rectifying column
Upside connect a static mixer be set, make mother solution containing aniline waste water mix from entering static mixer containing aniline waste water entrance
Closing, add liquid caustic soda mixing by alkali liquor inlet simultaneously and be neutralized in static mixer, after neutralization, aniline is by anilinechloride
Form be converted into aniline, consequently facilitating rectification.
In the present invention, the downside of described rectifying column is provided with steam inlet and condensation-water drain.
Live steam steam inlet on the downside of rectifying column is directly entered, and strips containing aniline waste water, strips heat exchange
The steam condensate of rear generation flows out from described condensation-water drain.
In the present invention, on described lithium bromide chiller condenser, the first described condenser and the second condenser respectively
It is connected with cooling water supply pipe and CWR.
As a preferred embodiment of the present invention, at the bottom of the tower of rectifying column of the present invention, it is connected with heat exchanger.
Containing heat from waste water out at the bottom of rectifying tower, if directly sending sewage treatment plant to process, will result in this part
The waste of heat.The present invention arranges a heat exchanger in connection at the bottom of rectifying tower, and at the bottom of such tower, waste water is collected by heat exchanger heat exchange
Enter back into sewage treatment plant after heat to process, thus avoid the waste of waste water heat at the bottom of tower.
Use the circulating device economic benefit for producing nigrosine provided by the present invention obvious, the least by rectifying tower top
Time produce 5310Kg low-pressure steam, replace 0.6MPa steam drive lithium bromide chiller produce 7 DEG C of cool water quantities be 500m3/ h, supply
Workshop refrigeration needs.Steam expense per ton presses 200 yuan of calculating, and the whole year can steam saving expense about 7,650,000.
Compared with prior art, present invention have the advantage that
(1) circulating device for producing nigrosine provided by the present invention can effectively process aniline black byestuffs waste water, real
The resource of existing pollutant and the cleaning of nigrosine produce, and the removal of aniline can reduce the murder by poisoning to biochemical wastewater treatment, for dirt
Large Water Treatment Field realizes qualified discharge and provides premise；Meanwhile, the aniline of recovery can return as the raw material of nigrosine and produce
Process cycles utilizes；
(2) circulating device for producing nigrosine provided by the present invention effectively utilize rectifying tower top aniline steam and
The gas-phase potential heat of steam, utilizes low-pressure steam to drive lithium bromide chiller condenser, produces 7 DEG C of water and freeze for each workshop,
12 DEG C of water it are converted into after each workshop reacting kettle jacketing or heat exchanger heat exchange, then after low-pressure steam drives lithium bromide chiller
Producing 7 DEG C of water to recycle, make the heat of rectifying column tower top comprehensively be effectively utilized, 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 circulating device schematic diagram for producing nigrosine provided by the present invention；
Wherein, in accompanying drawing, each component names is as follows:
1 storage tank, 2 feed preheaters, 3 rectifying columns, 4 condensers, 41 first condensers,
42 second condensers, 5 deckers, 6 lithium bromide chiller condensers, 7 static mixers, 8 change
Hot device, 9 cooling water supply pipes, 10 CWRs, 11 elevator pumps, 12 manganese sand filter,
13 ejectors, 14 flash tanks, 15 air coolers, 16 condensation reaction stills, 17 acidification reaction stills,
18 centrifuges.
Detailed description of the invention
Below in conjunction with accompanying drawing, the present invention is described in further detail.
Embodiment one
As it is shown on figure 3, the present embodiment provide a kind of circulating device for producing nigrosine, including condensation reaction still 16,
Acidification reaction still 17, rectifying column 3, condenser 4 and decker 5, wherein, between described acidification reaction still 17 and rectifying column 3
It is connected with centrifuge 18；Lithium bromide chiller condenser 6, institute it is connected with between described rectifying column 3 and described condenser 4
The lithium bromide chiller condenser 6 stated is provided with recirculated water entrance and circulating water outlet.
The present invention is connected between described acidification reaction still 17 and rectifying column 3 and arranges centrifuge 18, can make working environment
It is that total enclosing operates by open type operation adjustment, effectively prevents the volatilization of material, protect environment；Improve the operation ring of worker
Border.Meanwhile, the present invention effectively utilizes aniline steam and the gas-phase potential heat of water vapour of rectifying column 3 tower top, utilizes low-pressure steam to drive
Dynamic lithium bromide chiller condenser 6, produces 7 DEG C of water and freezes for each workshop, through each workshop reacting kettle jacketing or heat exchanger
It is converted into 12 DEG C of water after heat exchange, produces 7 DEG C of water after entering back into lithium bromide chiller condenser 6 condensation and recycle, make rectifying column 3 tower
The heat on top is comprehensively effectively utilized, and economic benefit is obvious.Meanwhile, strip through rectifying column 3 containing aniline waste water, lithium bromide machine
The aniline that group condenser 6 condenses, condenser 4 condenses and reclaims after decker 5 layering can return raw as the raw material of nigrosine
Production. art recycles.
In order to improve condensation effect further, condenser 4 of the present invention includes the first condenser 41 and the second condensation
Device 42, the first described condenser 41 and the second condenser 42 are connected to described lithium bromide chiller condenser 6 and layering in turn
Between device 5.
Described lithium bromide chiller condenser 6 is provided with aniline steam entry and aniline water out；Described aniline water
Steam inlet is connected by the tower top of pipeline with described rectifying column 3；Described aniline water out passes through pipeline with described
First condenser 41 is connected.
The upside of described rectifying column 3 is connected with static mixer 7.
One end of described static mixer 7 is provided with alkali liquor inlet and the entrance Han aniline waste water, the other end and described essence
The upside evaporating tower 3 is connected.
The original ph of the mother solution containing aniline waste water is acid, and aniline is presented in hydrochlorate, by rectifying column 3
Upside connect a static mixer 7 be set, make mother solution containing aniline waste water enter static mixer 7 from containing aniline waste water entrance
In, in static mixer 7, adding liquid caustic soda mixing by alkali liquor inlet simultaneously and be neutralized, after neutralization, aniline is by anilinechloride
Form be converted into aniline, consequently facilitating rectification.
The downside of described rectifying column 3 is provided with steam inlet and condensation-water drain.
Live steam steam inlet on the downside of rectifying column 3 is directly entered, and strips containing aniline waste water, strips heat exchange
The steam condensate of rear generation flows out from described condensation-water drain.
Connect respectively on described lithium bromide chiller condenser 6, the first described condenser 41 and the second condenser 42
It is provided with cooling water supply pipe 9 and CWR 10.
The work process of a kind of circulating device for producing nigrosine that the present embodiment is provided comprises the steps:
(1) catalyst, Nitrobenzol and aniline are put into condensation reaction still 16 carries out condensation reaction, obtain containing excessive benzene
The nigrosine product of amine；
(2) in acidification reaction still 17, hot water and 30% hydrochloric acid are added, by the aniline containing excess aniline of step (1) gained
Black product joins and carries out acidification reaction in acidification reaction still 17, and the product obtained is produced by the centrifugal nigrosine that obtains of centrifuge 18
Product and containing aniline waste water；
(3) static mixing is entered by pipeline from containing aniline waste water entrance and alkali liquor inlet respectively containing aniline waste water and alkali liquor
Mixing in device 7, send into rectifying column 3 tower top after mixing, steam steam inlet on the downside of rectifying column 3 is directly entered simultaneously, to containing
Aniline waste water strips, the waste water decontaminated water factory and office reason produced at the bottom of rectifying column 3 tower after stripping；
(4) after stripping, rectifying column 3 tower top produces aniline and the gas phase mixture entrance lithium bromide chiller condenser 6 of water are cold
Solidifying；Be simultaneously from 12 DEG C of recirculated waters in other workshops and enter lithium bromide chiller condenser 6 by recirculated water entrance, by aniline and
The gas-phase potential heat that the gas phase mixture of water produces drives lithium bromide chiller condenser 6 to form 7 DEG C of recirculated waters from circulating water outlet stream
Go out and freeze for other workshop, after each workshop reacting kettle jacketing or heat exchanger heat exchange, be converted into 12 DEG C of recirculated waters lead to again
Cross recirculated water entrance entrance lithium bromide chiller condenser 6 to recycle；
(5) gas phase mixture through lithium bromide chiller condenser 6 condensation becomes liquid phase mixture, passes sequentially through the first condensation
Device 41 and the second condenser 42 condense, and enter decker 5 and be layered after condensation, and upper strata aqueous phase contains a small amount of aniline,
Send static mixer 7 circulation by pipeline back to from the entrance containing aniline waste water and carry out the operation of step (3)；Lower floor's aniline is mutually as closing
The raw material becoming nigrosine returns production technology circulation and carries out the operation of step (1).
Embodiment two
The present embodiment is the further improvement to embodiment one, for reclaiming at the bottom of rectifying column 3 tower the heat of waste water out,
Connect at the bottom of the tower of described rectifying column 3 and a heat exchanger 8 is set.Containing heat from waste water out at the bottom of rectifying column 3 tower, if directly
Send sewage treatment plant to process, will result in the waste of this partial heat.The present invention arranges a heat exchanger 8 in connection at the bottom of rectifying column 3 tower,
So waste water at the bottom of tower first passes through and enters back into sewage treatment plant's process after heat is collected in heat exchanger 8 heat exchange, thus avoids at the bottom of tower useless
The waste of hydro-thermal amount.
Comparative example
Being contrasted by the device of assembly of the invention and prior art, the oldest device is the device of Fig. 1, improvement
Device is the device of Fig. 2.Result see table shown in 1:
Table 1, the new and old device of prior art contrast with the major economic indicators of assembly of the invention
On the one hand device provided by the present invention effectively utilizes aniline steam and the gas-phase potential heat of steam of rectifying tower top,
Utilize low-pressure steam to drive lithium bromide chiller condenser, produce 7 degree of cold water and freeze for other workshops each, anti-through each workshop
It is converted into the water of 12 degree after answering still chuck or heat exchanger heat exchange, then after low-pressure steam drives lithium bromide chiller, produces 7 degree
Water recycles, and makes the heat of rectifying column tower top comprehensively be effectively utilized, and economic benefit is obvious.By rectifying tower top per hour
Producing 5310Kg low-pressure steam, replacing 0.6MPa steam drive lithium bromide chiller to produce 7 DEG C of cool water quantities is 500m3/ h, supplies car
Between refrigeration need.Steam expense per ton presses 200 yuan of calculating, and the whole year can steam saving expense about 7,650,000.On the other hand, with old dress
The device put and improve is compared, and uses the circulating device of the present invention to greatly reduce the consumption of recirculated water.
As it has been described above, combine the plan content given by accompanying drawing, similar technical scheme can be derived.In every case it is not take off
From the content of technical solution of the present invention, any simple modification of above example being made according to the technical spirit of the present invention, etc.
With change and modification, all still fall within the range of technical solution of the present invention.
Claims (6)
1. for producing a circulating device for nigrosine, including condensation reaction still (16), acidification reaction still (17), rectifying column
(3), condenser (4) and decker (5), it is characterised in that described acidification reaction still (17) is connected between rectifying column (3)
It is provided with centrifuge (18)；It is connected with lithium bromide chiller condenser between described rectifying column (3) and described condenser (4)
(6), described lithium bromide chiller condenser (6) is provided with recirculated water entrance and circulating water outlet；Described rectifying column (3) upper
Side is connected with static mixer (7), and the downside of described rectifying column (3) is provided with steam inlet and condensation-water drain.
Circulating device the most according to claim 1, it is characterised in that described condenser (4) includes the first condenser
(41) and the second condenser (42), described the first condenser (41) and the second condenser (42) are connected to described bromination in turn
Between lithium train condenser (6) and decker (5).
Circulating device the most according to claim 2, it is characterised in that described lithium bromide chiller condenser (6) is provided with
Aniline steam entry and aniline water out；Described aniline steam entry is by the tower of pipeline with described rectifying column (3)
Top is connected；Described aniline water out is connected with described the first condenser (41) by pipeline.
Circulating device the most according to claim 1, it is characterised in that one end of described static mixer (7) is provided with alkali
Liquid entrance and the entrance Han aniline waste water, the other end is connected with the upside of described rectifying column (3).
Circulating device the most according to claim 2, it is characterised in that described lithium bromide chiller condenser (6), described
Cooling water supply pipe (9) and CWR it is connected with respectively on first condenser (41) and the second condenser (42)
(10)。
Circulating device the most according to claim 1, is connected with heat exchanger (8) at the bottom of the tower of described rectifying column (3).
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| WO2003022918A1 (en) * | 2001-09-06 | 2003-03-20 | Basf Aktiengesellschaft | Polyamide-based thermoplastic molding materials and single-piece and multiple-piece plastic shaped bodies made from said thermoplastic molding materials |
| WO2003091336A1 (en) * | 2002-04-26 | 2003-11-06 | Basf Aktiengesellschaft | Flame-resistant black thermoplastic moulded masses |
| CN101817791A (en) * | 2009-02-27 | 2010-09-01 | 严纪一 | Method for directly producing water soluble aniline black |
| CN101987816A (en) * | 2009-07-31 | 2011-03-23 | 宜兴市前成生物有限公司 | Waste heat comprehensive utilization device during the production process of fumaric acid |
| CN204454953U (en) * | 2015-01-13 | 2015-07-08 | 青岛双桃精细化工（集团）有限公司 | A kind of circulation device for the production of nigrosine |
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2015
- 2015-01-13 CN CN201510016605.4A patent/CN104610175B/en active Active
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2003022918A1 (en) * | 2001-09-06 | 2003-03-20 | Basf Aktiengesellschaft | Polyamide-based thermoplastic molding materials and single-piece and multiple-piece plastic shaped bodies made from said thermoplastic molding materials |
| WO2003091336A1 (en) * | 2002-04-26 | 2003-11-06 | Basf Aktiengesellschaft | Flame-resistant black thermoplastic moulded masses |
| CN101817791A (en) * | 2009-02-27 | 2010-09-01 | 严纪一 | Method for directly producing water soluble aniline black |
| CN101987816A (en) * | 2009-07-31 | 2011-03-23 | 宜兴市前成生物有限公司 | Waste heat comprehensive utilization device during the production process of fumaric acid |
| CN204454953U (en) * | 2015-01-13 | 2015-07-08 | 青岛双桃精细化工（集团）有限公司 | A kind of circulation device for the production of nigrosine |
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| 醇溶苯胺黑生产废水中苯胺的回收;王守恒.等;《化学工业与工程技术》;20090630;第30卷(第3期);第48-50页 * |
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