CN103964531A - Reverse micelle dye extraction and recycling method for textile dyeing waste water - Google Patents
Reverse micelle dye extraction and recycling method for textile dyeing waste water Download PDFInfo
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- CN103964531A CN103964531A CN201410209600.9A CN201410209600A CN103964531A CN 103964531 A CN103964531 A CN 103964531A CN 201410209600 A CN201410209600 A CN 201410209600A CN 103964531 A CN103964531 A CN 103964531A
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Abstract
The invention relates to a reverse micelle dye extraction and recycling method for textile dyeing waste water. According to the method, a reverse micelle extraction method is used for extracting anionic azo dye in dyeing waste water, and the dye is transferred to a new water phase through re-extraction for dyeing again. The method has the advantages of simpleness in preparation process, low cost, environmental friendliness, high safety and easiness in industrial implementation; more importantly, both the dye and n-pentanol can be reused after the dye in the dyeing waste water is treated by the reverse micelle extraction technology, so that the dye reuse rate is high; on one hand, the environmental pollution problem caused by dyeing waste water discharge is solved; on the other hand, the method has remarkable cost advantage.
Description
Technical field
The present invention relates to inverse micelle abstraction and the reuse method of dyeing waste-water processing technology field, particularly a kind of dyeing waste-water.
Background technology
Textile industry is one of department that China's discharge amount of industrial wastewater is larger, according to incompletely statistics, the waste water of annual discharge has exceeded 1,000,000,000 tons, occupy the prostatitis of China's discharged volume of industrial waste water, wherein dyeing waste water quantity discharged accounts for 80% left and right of textile waste, in dyeing waste water, contain high-enriched organics, once enter rivers, water body will consume a large amount of dissolved oxygens, dyestuff in waste water can absorb light, reduce water transparency, cause fish and other aquatic organism death, destroy water ecology balance, can cause coloured water body simultaneously, affect daylight projection, hinder aquatic organism growth, therefore the problem of environmental pollution of textile industry is mainly that water pollutes.The treatment technology of organic dyeing waste water had presented the development trend of diversification in recent years, and common treatment method of printing and dying wastewater mainly comprises the technology such as biological process, physisorphtion and chemical method both at home and abroad.Biological process is separated and is degraded pollutents such as Wastewater Dyes by effects such as the flocculation of biomass, absorption and biological degradations.Biological treatment is used widely in treatment of Organic Wastewater because having the features such as operation cost is low and economic and practical.Since 20 century 70s, domestic to dyeing waste water taking biological treatment as main, account for more than 80%, especially account for the overwhelming majority with aerobe facture.But because biological process is not high to Dye Wastewater Decolorization clearance, be generally 50% left and right, so in the time having relatively high expectations for effluent color dilution, need be aided with physics or chemical method is processed, cause technique more loaded down with trivial details.Organic waste water physical treatment method mainly comprises absorption method and embrane method, wherein applying maximum is absorption method, researchist uses the materials such as charcoal piece, wood, tripoli, sugarcane, activated carbon, slag and sugarcane ash effectively to adsorb dyestuff, and kinetics of adsorption has been carried out at length inquiring into.Although these adsorption methods are very effective for removing of dyestuff, except gac, most of sorbent material is all difficult to reuse.And for using gac as for sorbent material, this method is that the powder of the porous mass such as gac and clay or particle are mixed with waste water, or allow waste water pass through the filter bed being formed by its granular substance, make pollution substance in waste water be attracted on porous mass surface or be filtered and remove.This method is very effective to dissolved organic matter in removal water, but it can not remove colloid and hydrophobic dye in water, and it only has good absorption property to water-soluble dyes such as cationic dyestuff, substantive dyestuff, matching stain, reactive dyestuffs, use range has certain limitation, and its price is also very expensive.Membrane separation process is that a kind of aperture is the separation method of molecular size, and the method can separate colloidal particle with dissolve polymer, can effectively remove the inexpungible suspended substance of precipitation.But after making to handle in this way dyeing waste water, also need to adopt machinery or chemical process to remove impurity, to reduce the fouling of separatory membrane, thereby reduce running expense, therefore technique is more loaded down with trivial details, and price is also more expensive.In treatment of Organic Wastewater, use maximum chemical methods to mainly contain flocculence and chemical oxidization method two classes.Flocculence mainly contains coagulating sedimentation and two kinds of methods of coagulation air-float, its principle is by add flocculation agent in waste water, the pollutent that makes to be originally dissolved in waste water or be trickle suspended state is combined into larger particles under physics chemical action, thereby be easy to separate with water, finally reach and remove the object that is enriched in Pollutants in Wastewater, but this method makes dyestuff and flocculation agent form mixture, has limited reusing of dyestuff.Chemical oxidization method is the study hotspot of current treatment of dyeing wastewater, this method is normally taking hydrogen peroxide as oxygenant, make itself and iron ion be combined in (Fenton reagent) under ozone or uv irradiating the organic pollutants such as dyestuff are effectively decomposed, even thoroughly degrade mineralising and be converted into harmless inorganics (such as carbonic acid gas, water etc.).Although this method is very effective for the degraded of dyestuff, conventionally can only be used for the removal of water lower concentration dyestuff, and dyestuff in waste water can not be reused after being decomposed.
Summary of the invention
Object of the present invention is just to provide a kind of extraction of the reverse micelle dyestuff for textile dyeing waste water and reuse method, it separates anionic dyestuff after inverse micelle abstraction with the waste water that contains impurity, make dye transfer in the reverse micelle system of Pentyl alcohol, revert in new water by rear extraction liquid extraction again, for dyeing again.
The object of the invention is to realize by such technical scheme, concrete steps are as follows:
1) textile dyeing waste water is carried out to filtration treatment;
2) extraction before reverse micelle, to step 1) add front extraction liquid in water body after treatment, the volume ratio scope of dyeing waste-water and front extraction liquid is 3:1 to 1:3, and at room temperature it is fully stirred, make the mixing solutions static layering under action of gravity after stirring, be divided into aqueous phase layer and organic solution layer, in organic solution layer, be formed for reclaiming the reverse micelle of dyestuff; Described front extraction liquid is made up of cetyl trimethylammonium bromide and Pentyl alcohol, and weight ratio scope is 1:1500～1:2500;
3) aqueous phase layer after layering is discharged, change new water into, then add rear extraction liquid to organic solution layer, wait for that the dyestuff in reverse micelle returns in new water, form clean dye liquor; Described rear extraction liquid is succinate sodium 2-ethylhexyl, its weight and step 2) in the ratio range of Pentyl alcohol be 1:1500～1:2500;
4) with step 3) in clean dye liquor textiles is dyeed.
Further, step 2) described in the well-beaten time be 10 to 60 minutes.
Further, step 2) described in the static layering time be 10 to 60 minutes.
Further, step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:1500.
Further, step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:2500.
Further, step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:2000.
Further, step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:1500.
Further, step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:2500.
Further, step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:2000.
Owing to having adopted technique scheme, the present invention has advantages of as follows:
The present invention uses inverse micelle abstraction method to remove the anionic azo dyes in dyeing waste-water, then by stripping dye transfer to new water, for dyeing again.The present invention has advantages of that preparation technology is simple, with low cost, environmental protection, safe and industrializing implementation are held, dyestuff in what is more important dyeing waste-water dyestuff and Pentyl alcohol after inverse micelle abstraction technique is processed all can be reused, dyestuff repeat usage is high, the problem of environmental pollution that has solved on the one hand dyeing waste-water discharge, has significant cost advantage on the other hand.
Other advantages of the present invention, target and feature will be set forth to a certain extent in the following description, and to a certain extent, based on will be apparent to those skilled in the art to investigating below, or can be instructed from the practice of the present invention.Target of the present invention and other advantages can be realized and be obtained by specification sheets and claims below.
Brief description of the drawings
Brief description of the drawings of the present invention is as follows.
Fig. 1 is schematic flow sheet of the present invention;
Fig. 2 is inverse micelle abstraction principle schematic;
Fig. 3 is reverse micelle system structural representation;
Fig. 4 uses inverse micelle abstraction method graphic representation that removes to REACTIVE Red 195 under different dyes concentration;
Fig. 5 uses reverse micelle stripping process data collection figure to REACTIVE Red 195 under different dyes concentration;
Fig. 6 is the dyeing K/S graphic representation of inverse micelle abstraction reuse dyestuff to cotton fabric;
Fig. 7 is the dyeing of cotton fabric in conventional water-bath.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described.
Reverse micelle refers to surfactant-dispersed in continuous non-polar solvent, and the nano level stable aggregate of one of spontaneous formation in the time that its concentration exceedes threshold value as micelle-forming concentration CMC.Inverse micelle abstraction technique is the principle based on liquid-liquid extraction, comprises that extraction and back-extraction gets process.Surfactant layer between organic solvent phase and water two macroface interfaces is with contiguous extract molecule generation electrostatic attraction, then the reverse micelle that two interface formations contain extract, then be diffused in organic phase, realize the front extraction process of extraction of extract, finally by changing water condition, as pH value, ionic species or ionic strength, can make again extract from organic phase, turn back in water, realize the rear extraction process of reextraction of extract.The present invention is different from traditional treatment method of printing and dying wastewater, and the dyestuff in what is more important dyeing waste water dyestuff and organic solvent after inverse micelle abstraction technique is processed all can be reused, and have obvious cost advantage.
Front extraction liquid of the present invention is cetyl trimethylammonium bromide and Pentyl alcohol, and weight ratio is 1:1500～1:2500;
Rear extraction liquid is succinate sodium 2-ethylhexyl, and in consumption and front extraction liquid, the weight ratio of Pentyl alcohol is 1:1500～1:2500.
Reverse micelle of the present invention obtains its pool diameter through particle size analysis and is about 10～20nm, adopts conductivitimeter to obtain its specific conductivity at 0～1.0 μ s/cm, and its chemical stability is good, and HLB value is low, remarkable to the effect of extracting of dyestuff.
Concrete technology is:
1) textile dyeing waste water being carried out to filtration treatment, is mainly to remove the fiber fragment producing in the dyeing course of processing;
2) extraction before reverse micelle: first add extraction liquid in dyeing waste-water, and at room temperature it is fully stirred, then make mixing solutions static layering under action of gravity, now the anionic dyestuff in dyeing waste-water progress into organic solvent Pentyl alcohol under the electrostatic attraction effect of cats product cetyl trimethylammonium bromide in as shown in Figure 2, finally reach the object that dyestuff removes from dyeing waste-water, now dyestuff is mainly present in the reverse micelle system in solvent phase, as shown in Figure 3;
3) reverse micelle strip: first by step 2) in waste water change new tap water into, then in Pentyl alcohol, add anion surfactant succinate sodium 2-ethylhexyl, now the anionic dyestuff in reverse micelle system is subject to the effects such as the repulsion of anion surfactant and transfers in new water, reach gradually the object that dyestuff reclaims, the dyestuff that extraction liquid also can be re-used in next time simultaneously removes.
4) with the dyestuff reclaiming, the textiless such as wool, silk and cotton are dyeed, improve the utilization ratio of dyestuff.
Beneficial effect of the present invention is: use inverse micelle abstraction method to remove anionic azo dyes in dyeing waste water, these are different from traditional treatment method of printing and dying wastewater, there is preparation technology simple, with low cost, environmental friendliness, the advantages such as safe and industrializing implementation is easy, dyestuff in what is more important dyeing waste-water dyestuff and organic solvent after inverse micelle abstraction technique is processed all can be reused, dyestuff repeat usage is high, the method has reduced the problem of environmental pollution of dyeing waste water discharge on the one hand, there is on the other hand obvious cost advantage, therefore there is very vast potential for future development.
Embodiment 1
The present embodiment extracts the REACTIVE Red 195 dyeing waste-water of 100ml concentration 0.2g/L, front extraction liquid 300ml, and wherein in front extraction liquid and anti-stripping agent, each component is:
Front extraction liquid: cetyl trimethylammonium bromide and Pentyl alcohol, weight ratio is 1:2000;
Rear extraction liquid: succinate sodium 2-ethylhexyl, in consumption and front extraction liquid, the weight ratio of Pentyl alcohol is 1:2000.
Concrete steps are:
1) textile dyeing waste water being carried out to filtration treatment, is mainly to remove the fiber fragment producing in the dyeing course of processing;
2) extraction before reverse micelle: first add extraction liquid in dyeing waste-water, and at 15 degree temperature, it is fully stirred, churning time is 60 minutes, then make mixing solutions static layering under action of gravity, be 60 minutes rest time, now the anionic dyestuff in dyeing waste-water progress into organic solvent Pentyl alcohol under the electrostatic attraction effect of cats product cetyl trimethylammonium bromide in as shown in Figure 2, finally reach the object that dyestuff removes from dyeing waste-water, now dyestuff is mainly present in the reverse micelle system in solvent phase, as shown in Figure 3,
3) reverse micelle strip: first by step 2) in waste water change new tap water into, then in Pentyl alcohol, add anion surfactant succinate sodium 2-ethylhexyl, now the anionic dyestuff in reverse micelle system is subject to the effects such as the repulsion of anion surfactant and transfers in new water, waiting time is 60 minutes, reach gradually the object that dyestuff reclaims, the dyestuff that extraction liquid also can be re-used in next time simultaneously removes.
4) with the dyestuff reclaiming, the textiless such as wool, silk and cotton are dyeed, improve the utilization ratio of dyestuff.
In front extraction process, the removal rate of REACTIVE Red 195 reaches 99%; In rear extraction process, the rate of recovery that REACTIVE Red 195 is transferred to new water is 98%.
Embodiment 2
The present embodiment extracts the REACTIVE Red 195 dyeing waste-water of 100ml concentration 0.6g/L, front extraction liquid 165ml, and wherein in front extraction liquid and anti-stripping agent, each component is:
Front extraction liquid: cetyl trimethylammonium bromide and Pentyl alcohol, weight ratio is 1:1500;
Rear extraction liquid: succinate sodium 2-ethylhexyl, in consumption and front extraction liquid, the weight ratio of Pentyl alcohol is 1:1500.
Concrete steps are:
1) textile dyeing waste water being carried out to filtration treatment, is mainly to remove the fiber fragment producing in the dyeing course of processing;
2) extraction before reverse micelle: first add extraction liquid in dyeing waste-water, and at 25 degree temperature, it is fully stirred, churning time is 30 minutes, then make mixing solutions static layering under action of gravity, be 30 minutes rest time, now the anionic dyestuff in dyeing waste-water progress into organic solvent Pentyl alcohol under the electrostatic attraction effect of cats product cetyl trimethylammonium bromide in as shown in Figure 2, finally reach the object that dyestuff removes from dyeing waste-water, now dyestuff is mainly present in the reverse micelle system in solvent phase, as shown in Figure 3,
3) reverse micelle strip: first by step 2) in waste water change new tap water into, then in Pentyl alcohol, add anion surfactant succinate sodium 2-ethylhexyl, now the anionic dyestuff in reverse micelle system is subject to the effects such as the repulsion of anion surfactant and transfers in new water, waiting time is 30 minutes, reach gradually the object that dyestuff reclaims, the dyestuff that extraction liquid also can be re-used in next time simultaneously removes.
4) with the dyestuff reclaiming, the textiless such as wool, silk and cotton are dyeed, improve the utilization ratio of dyestuff.
In front extraction process, the removal rate of REACTIVE Red 195 reaches 91%; In rear extraction process, the rate of recovery that REACTIVE Red 195 is transferred to new water is 90%.
Embodiment 3
The present embodiment extracts the REACTIVE Red 195 dyeing waste-water of 100ml concentration 1.0g/L, front extraction liquid 30ml, and wherein in front extraction liquid and anti-stripping agent, each component is:
Front extraction liquid: cetyl trimethylammonium bromide and Pentyl alcohol, weight ratio is 1:2500;
Rear extraction liquid: succinate sodium 2-ethylhexyl, in consumption and front extraction liquid, the weight ratio of Pentyl alcohol is 1:2500.
Concrete steps are:
1) textile dyeing waste water being carried out to filtration treatment, is mainly to remove the fiber fragment producing in the dyeing course of processing;
2) extraction before reverse micelle: first add extraction liquid in dyeing waste-water, and at 35 degree temperature, it is fully stirred, churning time is 10 minutes, then make mixing solutions static layering under action of gravity, be 10 minutes rest time, now the anionic dyestuff in dyeing waste-water progress into organic solvent Pentyl alcohol under the electrostatic attraction effect of cats product cetyl trimethylammonium bromide in as shown in Figure 2, finally reach the object that dyestuff removes from dyeing waste-water, now dyestuff is mainly present in the reverse micelle system in solvent phase, as shown in Figure 3,
3) reverse micelle strip: first by step 2) in waste water change new tap water into, then in Pentyl alcohol, add anion surfactant succinate sodium 2-ethylhexyl, now the anionic dyestuff in reverse micelle system is subject to the effects such as the repulsion of anion surfactant and transfers in new water, waiting time is 10 minutes, reach gradually the object that dyestuff reclaims, the dyestuff that extraction liquid also can be re-used in next time simultaneously removes.
4) with the dyestuff reclaiming, the textiless such as wool, silk and cotton are dyeed, improve the utilization ratio of dyestuff.
In front extraction process, the removal rate of REACTIVE Red 195 reaches 81%; In rear extraction process, the rate of recovery that REACTIVE Red 195 is transferred to new water is 78%.
The dyeing water body that the present invention is reclaimed is for cotton fabric dyeing process, first will be placed in 50ml and specify the aqueous dye solutions of dye strength through pretreated about 1.0g cotton fabric, start into dying at 55 DEG C, dye and after 10 minutes, add 50% sodium-chlor, the continuous sodium-chlor that adds again 50% after 15 minutes that dyes, then after dyeing again 15 minutes, add the sodium carbonate of normality to carry out fixation, fixation was taken out sample after 30 minutes, with cold water washing, soap boiling, washing and oven dry, finally adopt computer colour matching instrument to measure the colored surfaces degree of depth K/S curve of dyed cotton fabric, as shown in Figure 6.
Finally explanation is, above embodiment is only unrestricted in order to technical scheme of the present invention to be described, although the present invention is had been described in detail with reference to preferred embodiment, those of ordinary skill in the art is to be understood that, can modify or be equal to replacement technical scheme of the present invention, and not departing from aim and the scope of the technical program, it all should be encompassed in the middle of claim scope of the present invention.
Claims (9)
1. for the extraction of reverse micelle dyestuff and the reuse method of textile dyeing waste water, it is characterized in that, concrete steps are as follows:
1) textile dyeing waste water is carried out to filtration treatment;
2) extraction before reverse micelle, to step 1) add front extraction liquid in water body after treatment, the volume ratio scope of dyeing waste-water and front extraction liquid is 3:1 to 1:3, and at room temperature it is fully stirred, make the mixing solutions static layering under action of gravity after stirring, be divided into aqueous phase layer and organic solution layer, in organic solution layer, be formed for reclaiming the reverse micelle of dyestuff; Described front extraction liquid is made up of cetyl trimethylammonium bromide and Pentyl alcohol, and weight ratio scope is 1:1500～1:2500;
3) aqueous phase layer after layering is discharged, change new water into, then add rear extraction liquid to organic solution layer, wait for that the dyestuff in reverse micelle returns in new water, form clean dye liquor; Described rear extraction liquid is succinate sodium 2-ethylhexyl, its weight and step 2) in the ratio range of Pentyl alcohol be 1:1500～1:2500;
4) with step 3) in clean dye liquor textiles is dyeed.
2. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 2) described in the well-beaten time be 10 to 60 minutes.
3. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 2) described in the static layering time be 10 to 60 minutes.
4. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:1500.
5. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:2500.
6. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 2) described in before the cetyl trimethylammonium bromide of extraction liquid and the weight ratio scope of Pentyl alcohol be 1:2000.
7. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:1500.
8. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:2500.
9. the reverse micelle dyestuff for textile dyeing waste water as claimed in claim 1 extraction and reuse method, is characterized in that step 3) described in the weight ratio of succinate sodium 2-ethylhexyl and Pentyl alcohol be 1:2000.
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| CN105923681B (en) * | 2016-06-16 | 2019-04-30 | 江苏大学 | A kind of method of fluorescent whitening agent VBL in cloud point extraction sewage |
| CN111732322A (en) * | 2020-07-10 | 2020-10-02 | 同济大学 | Sludge deep dehydration treatment technical method for recycling conditioner |
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