CN107337246A - Reactive dyeing raffinate recovery system and recovery method - Google Patents
Reactive dyeing raffinate recovery system and recovery method Download PDFInfo
- Publication number
- CN107337246A CN107337246A CN201710711114.0A CN201710711114A CN107337246A CN 107337246 A CN107337246 A CN 107337246A CN 201710711114 A CN201710711114 A CN 201710711114A CN 107337246 A CN107337246 A CN 107337246A
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- Prior art keywords
- extraction
- raffinate
- extractant
- organic solvent
- reactive
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Classifications
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/26—Treatment of water, waste water, or sewage by extraction
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/30—Nature of the water, waste water, sewage or sludge to be treated from the textile industry
Abstract
A kind of reactive dyeing raffinate recovery system, including extracting system and back extraction system are provided；Reactive dye in raffinate are extracted in organic solvent by the extracting system, and the raffinate after extraction is used to dye；And the back extraction system active dyestuff will be extracted in the extracting system organic solvent in reactive dye be stripped into the aqueous solution, the organic solvent after back extraction is back to extracting system as extractant.A kind of recovery method is also disclosed, Centrifugical extraction isolation technics of the present invention is a kind of polar organic matter chemical extraction separation method based on reversible reaction, the closed loop cycle of two systems of water+salt and extractant is formd in the processing procedure to dyeing residual liquid, interacted in centrifugal extraction apparatus, continuity the hydrolised dye in dyeing residual liquid is extracted, so that the raffinate containing high salinity is recycled, a large amount of discharges of salt are avoided.Both reduce the pollution to environment, and reduce production cost again.
Description
Technical field
The present invention relates to textile printing and dyeing field, and in particular to textile printing and dyeing wastewater processing and recovery.
Background technology
The dyeing waste water that China is discharged every year is up to 2,000,000,000 tons, and wherein vital staining waste water accounts for 20% or so, total amount about 400,000,000
Ton.
, to obtain good washing fastness due to being generated in Dyeing with Reactive Dyes with substantial amounts of hydrolised dye
Hydrolised dye is thoroughly removed, therefore, the precursor structure of reactive dye is designed to have relatively low affinity to fiber, while
The salt that 1-10% must be added during vital staining promotees dye, more to some deep dense color dosages to improve the dye-uptake of dyestuff
Up to 1 ton of salt/ton fiber, these salt are lossless in dyeing, directly all discharged from sewage after dyeing, many factory's day salt discharges
Amount exceedes tens of tons, national 1,000,000 tons of annual emissions salt dosage, such discharge year in year out, soil, river to surrounding
Ecology cause to seriously endanger.
The content of the invention
In order to overcome drawbacks described above, the present invention provides a kind of reactive dyeing raffinate recovery system and recovery method.
A kind of reactive dyeing raffinate recovery system, including extracting system and back extraction system；The extracting system will be residual
Reactive dye in liquid are extracted in organic solvent, and the raffinate after extraction is used to dye；And the back extraction system is by institute
The reactive dye stated in the organic solvent that active dyestuff is extracted in extracting system are stripped into the aqueous solution, having after back extraction
Solvent is back to extracting system as extractant.
The extracting system and back extraction system are Centrifugical extraction.
It is 1-2 by volume that extractant in the extracting system, which is,:1-2:3-5 trioctylamine, n-octyl alcohol and diesel oil
Mixture.
Aqueous phase extractant in the back extraction system is the alkaline solution that pH is 10-11.5. a kind of reactive dyeing is residual
Liquid recovery method, comprises the following steps：S1, raffinate, the hydrolysed reactive dye in raffinate is extracted in organic solvent, extracted
The aqueous solution of rear saliferous is taken to be re-used for dyeing；S2, by being stripped reactive dye in the organic solvent for extracting active dyestuff
It is extracted to aqueous phase；And S3, recycled extractant is used as by the organic solvent after back extraction.
Also include pre-treatment step before the S1 steps, the pre-treatment step is the pH of dyeing residual liquid to be adjusted with acid
It is whole to arrive 2-3.
The acid is at least one of sulfuric acid, formic acid, acetic acid.
The extraction and back extraction are Centrifugical extraction.
It is 1-2 by volume that the extractant of the extraction, which is,:1-2:The mixture of 3-5 trioctylamine, n-octyl alcohol and diesel oil.
The aqueous phase extractant of the back extraction is the alkaline solution that pH is 10-11.
Centrifugical extraction isolation technics of the present invention is a kind of polar organic matter chemical extraction based on reversible reaction
Separation method, the closed loop cycle of two systems of water+salt and extractant is formd in the processing procedure to dyeing residual liquid, is being centrifuged
Interact in extraction equipment, extract the hydrolised dye in dyeing residual liquid to continuity, so that containing the residual of high salinity
Liquid is recycled, and avoids a large amount of discharges of salt.Both reduce the pollution to environment, and reduce production cost again.Simultaneously
Remove more than 95% pollutant such as hydrolised dye, extractant used can recycling utilization, and realize industrialization should
With；Regenerant salt Water Sproading reactive dyeing process technology is developed, solves the high chroma of reactive dyeing, high salinity is given up
Water process problem, the recycling of dyeing residual liquid salt and water is realized, breach the existing reactive dyeing mode of production
Ecology and environmental constraints.
Brief description of the drawings
Its example embodiment is described in detail by referring to accompanying drawing, above and other feature and advantage of the invention will become
It is more obvious.
Fig. 1 is the reactive dyeing raffinate recovery system schematic diagram of the present invention；
Fig. 2 is the structural representation of the reactive dyeing raffinate recovery system of the present invention；And
Fig. 3 is the reactive dyeing raffinate recovery system schematic diagram of the present invention.
Wherein, description of reference numerals is as follows：
1- extractant batch tanks；2- raffinate storage tanks；3- flowmeters；4- back washing agent storage tanks；5- back washing agent batch tanks；6- is extracted
Agent recycling can；7- pumps；8- three-level counterflow extraction devices；9- two level counterflow extraction devices.
Embodiment
The present invention is elaborated with reference to embodiment.
The reactive dyeing raffinate recovery system of the present invention, including extracting system and back extraction system.Extracting system will be residual
Reactive dye in liquid are extracted in organic solvent, and the raffinate after extraction is used to dye.Back extraction system is by extracting system
The reactive dye extracted in the organic solvent of active dyestuff are stripped into the aqueous solution, and the organic solvent after back extraction is back to extraction
System is taken as extractant.
The reactive dyeing raffinate recovery method of the present invention, comprises the following steps：S1, raffinate, by raffinate
Reactive dye are extracted in organic solvent, and the aqueous solution of saliferous is re-used for dyeing after extraction；S2, extraction there is into work by being stripped
Reactive dye are extracted to aqueous phase in the organic solvent of property dyestuff；And S3, extractant will be used as by the organic solvent after back extraction
Recycle.
Also include pre-treatment step before S1 steps, it with the pH value of acid adjustment raffinate is 2-3 that pre-treatment step, which is,.To residual
Liquid acid adjustment processing is in order to which in extraction process, extractant is changed into cation by non-ionic state, is lived with being complexed in raffinate
Property the anion that hydrolyzes to form of dyestuff realize the purpose that dyestuff is extracted from raffinate.Acid used can be inorganic acid, can also
It is organic acid, such as inorganic acid can be sulfuric acid etc., organic acid can be formic acid, acetic acid etc..Choosing the extraction of extracting system
During agent, typically require extractant can not be dissolved each other with raffinate, to the solubility of reactive dye much larger than reactive dye in raffinate
Solubility, to be not easy to volatilize and be unable to raffinate to react.Consider factors above, not volatile organic molten of generally use
Agent should select appropriate organic solvent as extractant according to the species of reactive dye.Can in extractant in the present invention
With including complexing agent, cosolvent and diluent.Complexing agent in extraction process in extractant is in acid condition by nonionic shape
State is changed into cation, to be complexed the mesh that the anion that hydrolysis of reactive dye is formed in raffinate realizes the extraction dyestuff from raffinate
's.Cosolvent is the good solvent of selected complexing agent and complexing product, in favor of the formation and phase transfer of complex compound.Diluent is used for
Improve viscosity, surface tension of mixed extractant etc., improve the effect of extracting power.Those skilled in the art can be according to selected
Complexing agent selects suitable cosolvent and diluent on demand.Reactive dye are a kind of water-soluble dyes with active group,
It can occur with the hydroxyl on cellulose fibre, the amino on protein fibre, the amino on Fypro and carboxylic hydroxyl covalent
Bond is closed, therefore also known as chemically-reactive dyes.Reactive dye are distinguished with differential responses base, mainly there is nine types, i.e. dichloro three
Piperazine type, a chloro-s-triazine type, Vinyl-Sulfone Type, a chloro-s-triazine and vinyl sulfone double-active base, double chloro-s-triazine A types, double chlorine
S-triazine Type B, phosphonic acids its type, the chlorine pyrimidine Type of difluoro one and picolinic acid triazine fundamental mode.Because different types of reactive dye exist
All it is negatively charged after hydrolysis, therefore the complexing agent selection in extractant can form the organic molten of cation in acid condition
Agent, such as tertiary amines or its mixture, can be that different ratios is mixed to form the mixed extractant R containing polyamine3N.With
Under use sulfuric acid when acid adjustment is handled exemplified by, illustrate extraction of the extractant to hydrolised dye in raffinate for including polyamine
Journey：
As shown in formula (1), polyamine is changed into cation by non-ionic state in acid condition.
As shown in formula (2), cation and the dyestuff R ' SO of hydrolysis3Complexing.
Purpose in extractant is extracted into so as to realize dyestuff from raffinate.
Extractant may be, but not limited to, and be by volume 1-2:1-2:3-5 trioctylamine, n-octyl alcohol and diesel oil it is mixed
Compound.Those skilled in the art can suitably select other suitable extractants according to the design of the present invention.
Back washing agent system is that the dyestuff being extracted into organic solvent is stripped into aqueous phase.Aqueous phase extractant can be added
PH value is 10-11 alkaline aqueous solution, and alkaline aqueous solution can be sodium hydrate aqueous solution.After extraction process, in oil phase
The complex compound of formation removes H under alkaline conditions+, it is non-ionic state that extractant, which is replied, makes hydrolised dye and separation of oil, is entered
Aqueous phase dissolved, complete back extraction.Back extraction process such as formula (3)：
Organic solvent after back extraction is back to extracting system as extractant.
Extraction and back extraction can use Centrifugical extraction.
Fig. 1 is reactive dyeing raffinate recovery system schematic diagram.Overflow dyeing machine excludes raffinate, and raffinate is entered to collect and adjusted
Acid, then the raffinate supply centrifugal extraction apparatus of collection is extracted, the raffinate after extraction is salt-containing solution, can be returned
Overflow dyeing machine reuses；Then the organic solvent for extracting dyestuff is stripped, dyestuff therein is stripped to aqueous phase, is stripped
Organic solvent be supplied to centrifugal extraction apparatus to be reused as extractant.
Fig. 2 is the structural representation of reactive dyeing raffinate recovery system.Reactive dyeing raffinate recovery system bag
Include extractant batch tank 1, raffinate storage tank 2, the three-level counterflow extraction device 8 for extraction, the two level counter-current extraction for back extraction
Device 9, back washing agent batch tank 5, back washing agent storage tank 4, extractant storage tank 6, the flowmeter 3 and pump 7 for controlling flow.Wherein this is
System extraction is made up of three identical centrifugal devices, such as can be commercially available model RYD680P, treating capacity 150m3/ h from
Center device, raffinate continue through three identical centrifugal devices, and continuous extraction is three times.Three-level counterflow extraction device is merely to solution
The present invention is released, the present invention is not limited to three-level counterflow extraction device, can also be other extraction equipments.The reasons why same,
Back extraction is also not limited to two level counterflow extraction device, can also be other extraction equipments.The system described in detail below
Raffinate removal process.It is possible, firstly, to be pre-processed to the waste liquid of overflow dyeing machine discharge, the pH for adjusting raffinate is 2-3.After pretreatment
Raffinate be stored in raffinate storage tank 2, by flowmeter 3 control raffinate enter three-level counterflow extraction device 8 raffinate flow, pass through
Raffinate after extraction is flowed out from extraction equipment, and decolouring salt solution is handled, and first adjusts pH to neutrality, then salt solution expected from being adjusted to is dense
Degree, to reuse.Organic solvent as extractant is stored in extractant batch tank 1, by the control of flowmeter 3 with
The opposite direction of the inflow direction of raffinate enters three-level counterflow extraction device 8, the reactive dye in raffinate.In three stage countercurrents
In extraction equipment 8, the flow direction of raffinate and the flow direction of extractant on the contrary, in order to quickly mix, scattered two phase liquid, obtain them
To sufficient mass transport process.The organic solvent of the active dyestuff of extraction flowed out from three-level counterflow extraction device 8 enters two level
In counterflow extraction device 9.Aqueous phase extractant for back extraction is sodium hydrate aqueous solution, pH value 10-11.Configured in back washing agent
Sodium hydroxide and water are hybridly prepared into sodium hydrate aqueous solution in tank 5, are then sent into sodium hydrate aqueous solution by pump 7 anti-
Extract in agent storage tank 7.Sodium hydrate aqueous solution in back washing agent storage tank 7 is by the control of flowmeter 3 with extracting active dyestuff
The stream of organic solvent flow into the opposite direction in two level counterflow extraction device 9, the complex compound of formation is gone under alkaline conditions
Except H+, it is non-ionic state that extractant, which is replied, makes hydrolised dye and separation of oil, into aqueous phase dissolved, completes back extraction.It is organic
Solvent is discharged from device 12, is flowed into extractant storage tank 6, for recycling.
Embodiment 1
As shown in Figures 2 and 3, discharged in the intake-outlet of each overflow dyeing machine of loose wool dyeing workshop (such as 1#-10# overflow dyeing machines)
It is special recovery and the pipeline that feeds intake, the vital staining raffinate of each dye vat is directly discharged in specific collecting pit M, through G1,
After G2 acid adjustments, into centrifugation decolouring system 2, raffinate is controlled into the raffinate stream of three-level counterflow extraction device 8 by flowmeter 3
Amount, the raffinate after extraction are exited into G3, G4 storage tank from centrifugal extraction apparatus 11, and it is dense to concentrate on progress salt solution in N ponds
Degree adjustment, to reuse.Organic solvent as extractant is stored in extractant batch tank 1, passes through the control of flowmeter 3
Three-level counterflow extraction device 8 is entered with the direction opposite with the inflow direction of raffinate, the hydrolysed reactive dye in raffinate.
In three-level counterflow extraction device 8, the flow direction of raffinate and the flow direction of extractant are on the contrary, being to quickly mix, scattered two mixing
Liquid, them is obtained sufficient mass transport process, improve extraction efficiency.The extract countercurrently gone out from three-level counterflow extraction device 8
Into in two level counterflow extraction device 9.Sodium hydrate aqueous solution pH value 10 for back extraction.By hydrogen in back washing agent batch tank 5
Sodium oxide molybdena and water are mixedly configured into sodium hydrate aqueous solution, and sodium hydrate aqueous solution then is sent into back washing agent storage tank 7 by pump 7
In.Sodium hydrate aqueous solution in back washing agent storage tank 7 is by the control of flowmeter 3 with the organic solvent with extracting active dyestuff
Stream flow into the opposite direction in two level counterflow extraction device 9, the complex compound of formation is removed into H under alkaline conditions+, extractant
Reply as non-ionic state, make hydrolised dye and separation of oil, into aqueous phase dissolved, complete back extraction.The hydrolysis being extracted out
Reactive dye are discharged from two level counterflow extraction device 10, and organic solvent is flowed into extractant storage tank 6 from 12 outlets, for sharp again
With.
Centrifugical extraction isolation technics of the present invention is a kind of polar organic matter chemical extraction based on reversible reaction
Separation method, the closed loop cycle of two systems of water+salt and extractant is formd in the processing procedure to dyeing residual liquid, is being centrifuged
Interact in extraction equipment, extract the hydrolised dye in dyeing residual liquid to continuity, so that containing the residual of high salinity
Liquid is recycled, and avoids a large amount of discharges of salt.Both reduce the pollution to environment, and reduce production cost again.Simultaneously
Remove more than 95% pollutant such as hydrolised dye, extractant used can recycling utilization, and realize industrialization should
With；Regenerant salt Water Sproading reactive dyeing process technology is developed, solves the high chroma of reactive dyeing, high salinity is given up
Water process problem, the recycling of dyeing residual liquid salt and water is realized, breach the existing reactive dyeing mode of production
Ecology and environmental constraints.
Certainly, the present invention can also have other various embodiments, ripe in the case of without departing substantially from spirit of the invention and its essence
Know those skilled in the art when can be made according to the present invention it is various it is corresponding change and deformation, but these corresponding change and become
Shape should all belong to the protection domain of appended claims of the invention.
Claims (10)
1. a kind of reactive dyeing raffinate recovery system, including extracting system and back extraction system；
Reactive dye in raffinate are extracted in organic solvent by the extracting system, and the raffinate after extraction is used to dye；
And
Reactive dye in the back extraction system will extract active dyestuff organic solvent in the extracting system are stripped to water
In solution, the organic solvent after back extraction is back to extracting system as extractant.
2. reactive dyeing raffinate recovery system according to claim 1, it is characterised in that the extracting system and anti-
Extraction system is Centrifugical extraction.
3. reactive dyeing raffinate recovery system according to claim 1, it is characterised in that in the extracting system
It is 1-2 by volume that extractant, which is,:1-2:The mixture of 3-5 trioctylamine, n-octyl alcohol and diesel oil.
4. reactive dyeing raffinate recovery system according to claim 1, it is characterised in that in the back extraction system
Aqueous phase extractant is the alkaline solution that pH is 10-11.
5. a kind of reactive dyeing raffinate recovery method, comprises the following steps：
S1, raffinate, the hydrolysed reactive dye in raffinate is extracted in organic solvent, the aqueous solution of saliferous is again after extraction
For dyeing；
S2, reactive dye in the organic solvent for extracting active dyestuff are extracted to aqueous phase by being stripped；And
S3, recycled extractant is used as by the organic solvent after back extraction.
6. recovery method according to claim 5, it is characterised in that also include pretreatment step before the S1 steps
Suddenly, the pre-treatment step is that the pH of dyeing residual liquid is adjusted into 2-3 with acid.
7. recovery method according to claim 6, it is characterised in that the acid is at least one in sulfuric acid, formic acid, acetic acid
Kind.
8. recovery method according to claim 5, it is characterised in that the extraction and back extraction are Centrifugical extraction.
9. recovery method according to claim 5, it is characterised in that it is 1-2 by volume that the extractant of the extraction, which is,:
1-2:The mixture of 3-5 trioctylamine, n-octyl alcohol and diesel oil.
10. recovery method according to claim 5, it is characterised in that the aqueous phase extractant of the back extraction is that pH is 10-11
Alkaline solution.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710711114.0A CN107337246A (en) | 2017-08-18 | 2017-08-18 | Reactive dyeing raffinate recovery system and recovery method |
| PCT/CN2018/087412 WO2019033805A1 (en) | 2017-08-18 | 2018-05-18 | Recovering system and method for reactive dye dyeing residual liquid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710711114.0A CN107337246A (en) | 2017-08-18 | 2017-08-18 | Reactive dyeing raffinate recovery system and recovery method |
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| CN107337246A true CN107337246A (en) | 2017-11-10 |
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| CN201710711114.0A Pending CN107337246A (en) | 2017-08-18 | 2017-08-18 | Reactive dyeing raffinate recovery system and recovery method |
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| WO (1) | WO2019033805A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109276910A (en) * | 2018-10-26 | 2019-01-29 | 新疆神邦环境工程有限公司 | A kind of continuous back extraction system |
| WO2019033805A1 (en) * | 2017-08-18 | 2019-02-21 | 新疆如意纺织服装有限公司 | Recovering system and method for reactive dye dyeing residual liquid |
| CN110552139A (en) * | 2018-05-30 | 2019-12-10 | 海宁绿宇纺织科技有限公司 | Method for recovering non-aqueous medium in disperse dye non-aqueous medium dyeing process |
| CN110627260A (en) * | 2019-10-25 | 2019-12-31 | 新疆神邦环境工程有限公司 | Dyeing raffinate salt recycling system |
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| CN110552139A (en) * | 2018-05-30 | 2019-12-10 | 海宁绿宇纺织科技有限公司 | Method for recovering non-aqueous medium in disperse dye non-aqueous medium dyeing process |
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Also Published As
| Publication number | Publication date |
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| WO2019033805A1 (en) | 2019-02-21 |
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Application publication date: 20171110 |