CN104313919A - Non-ionic mixed reversed micelles and preparation method thereof - Google Patents
Non-ionic mixed reversed micelles and preparation method thereof Download PDFInfo
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Abstract
The invention discloses non-ionic mixed reversed micelles and a preparation method thereof. The non-ionic mixed reversed micelles comprise the following components in percentage by mass: 2 to 12 percent of TX-100, 1 to 10 percent of Span, 10 to 35 percent of n-octyl alcohol, 30 to 60 percent of isooctane, 0.01 to 0.07 percent of dye, and 0.1 to 6.0 percent of distilled water. By taking the non-ionic mixed reversed micelles disclosed by the invention as a medium, fibers can obtain better dyeing performance; under the condition of the same dye using amount, the K/S value and the fastness of a dyeing product are obviously higher than the corresponding parameters of a conventional water bath dyeing product; more importantly, the non-ionic mixed reversed micelles system disclosed by the invention has the advantages of high chemical stability and high reusability; the dyeing water consumption can be greatly reduced, low-temperature dyeing of protein fibers can be realized, and the purposes of saving energy and reducing emission are achieved; salt-free dyeing of cellulose fibers can also be realized; moreover, the preparation process is simple; special equipment is not required; the preparation process is easy to operate; the industrialization and promotion prospects are bright.
Description
Technical field
The present invention relates to a kind of textile dyeing method, particularly a kind of nonionic Mixed reverse micelles and preparation method thereof.
Background technology
Textile printing and dyeing industry is one of industrial department that water consumption and quantity of wastewater effluent are very large.According to incompletely statistics, China's dyeing waste water discharge capacity is about 3 × 10 every day
6~ 4 × 10
6m
3printing and dyeing mill often processes 100 meters of fabrics, 3 ~ 5 tons of waste water can be produced, so the environmental destruction caused and economic loss are difficult to the appraisal, and the DYE PRODUCTION level of China and external gap larger, dyestuff dye-uptake is low, and auxiliary agent dosage is comparatively large, and this more increases the pollutional load of textile printing and dyeing industry.Containing functional groups such as a large amount of aromatic rings and amino in dye molecule, make waste component complexity and colourity deeply, great threat is produced to natural environment and health.
Along with the cry of various circles of society to environmental protection is more and more higher, scholars propose various new water saving dyeing in succession, main purpose use other dyeing medium to substitute whole or in part in traditional handicraft exactly adopt aqueous media, make whole dyeing course have no water or little water, become an important directions of staining technique development at present.Current supercritical fluid dyeing is paid close attention to widely due to the use and receiving avoiding water, the method emphasizes DISPERSE DYES to be dissolved in supercritical carbon dioxide fluid, system step-down is made after having dyeed, carbon dioxide is separated in gaseous form, residual dye then in solid form separate out and reusable, reach non-aqueous dyeing object.But high-tension apparatus has very high danger needed for this colouring method, dye with high costs.Occur that a kind of reverse micelle that adopts is as the textile dyeing method of dyeing medium in recent years, water-saving is energy-conservation owing to having for this method, environmental friendliness and security advantages of higher be subject to people and more and more paid close attention to.
Reverse micelle is by a kind of nano level stable aggregate of surfactant-dispersed spontaneous formation in continuous non-polar solven, the spherical polarity core wherein formed by surfactant hydrophilic group can not only a certain amount of water of solubilising or the aqueous solution, and effectively can limit existence and the interaction of its Middle molecule or ion.Usually reverse micelle can be divided into ion-type and the large class of nonionic two according to the character of surfactant.In recent years, the people such as external Sawada has used succinic acid two (2-ethylhexyl) ester sodium sulfonate (being called for short AOT) anionic reverse micelle to carry out Study on dyeing as medium to fiber.But result shows, the polarity of ionic group to pond of surfactant has adverse influence, and the pond in the unstable polarity core formed limits the application of this ion-type reverse micelle.Experiment proves that the reverse micelle system be made up of nonionic surface active agent then can overcome this shortcoming, for the physical-chemical reaction of compound in pond provides comparatively stable microenvironment.The nonionic reverse micelle that it is surfactant that Present Domestic has been prepared with OPEO (being called for short TX-100), and be applied in the dyeing of real silk or wool fibre, and achieve good effect.But the preparation of this reverse micelle is more difficult, and HLB value is higher, and ACID DYES is that the dyeability of medium to protein fibre is poor with it, thus have impact on applying of this technology.
Summary of the invention
In view of this, the object of this invention is to provide a kind of nonionic Mixed reverse micelles and preparation method thereof, ACID DYES and REACTIVE DYES is used to carry out the dyeing of protein fibre and cellulose fibre respectively, to solve the shortcoming existing for traditional water bath dyeing to adopt this reverse micelle as medium.
Nonionic Mixed reverse micelles of the present invention, comprises by mass percentage:
TX-100 (that is: Triton X-100, Value 3608): 2-12%,
Span (that is: sorbitan fatty acid ester class surfactant): 1-10%,
N-octyl alcohol: 10-35%,
Isooctane: 30-60%,
Dyestuff: 0.01-0.07%,
And distilled water: 0.1-6.0%.
The preparation method of nonionic Mixed reverse micelles of the present invention, comprises the following steps:
1) isooctane of certain mass, is taken at ambient temperature in dry beaker, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, in beaker, add TX-100, Span and the n-octyl alcohol of respective quality successively, finally use magnetic stirring apparatus to carry out rapid stirring to obtain flaxen mixing material to it;
2), aqueous dye solutions preparation: first take the ACID DYES of certain mass or REACTIVE DYES in the beaker of drying, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, the distilled water adding respective quality in beaker makes it to dissolve completely and obtains transparent aqueous dye solutions, regulate the pH value of aqueous dye solutions, with applicable reactive dyeing cellulose fibre or acid dyeing protein fibre;
3), then according to the mass ratio of composition each in nonionic Mixed reverse micelles, above-mentioned aqueous dye solutions implantation step 1 by respective volume) in preparation mixing material in obtain milky mixt, carry out ultrasonic wave process again after using magnetic stirring apparatus to stir milky mixt at ambient temperature, make it the nonionic Mixed reverse micelles system becoming transparence.
Beneficial effect of the present invention:
A kind of nonionic Mixed reverse micelles of the present invention and preparation method thereof, nonionic Mixed reverse micelles can make fiber obtain better dyeability as medium, and under identical dye dosage condition, the K/S value of dyeing and fastness are apparently higher than the relevant parameter of traditional water bath dyeing; The more important thing is, nonionic Mixed reverse micelles system of the present invention has the advantage that chemical stability is high and reusing is good, dyeing water consumption can not only be reduced significantly, realize the low temperature dyeing of protein fibre, reach the target of energy-saving and emission-reduction, also can realize the salt-free dyeing of cellulose fibre, and preparation technology is simple, do not need special installation, easily operate, industrialization promotion has a bright future.
Accompanying drawing explanation
Fig. 1 adopts nonionic Mixed reverse micelles of the present invention and existing non-ionic reverse micelle and conventional water-bath to be the K/S curve map of medium dyeing processes, a in figure: conventional water-bath dyeing, b: conventional water-bath dyeing+sodium chloride, c:TX-100 reverse micelle dyes, d:TX-100/Span40 Mixed reverse micelles dyeing (1:2);
Fig. 2 adopts nonionic Mixed reverse micelles of the present invention and existing non-ionic reverse micelle and conventional water-bath to be the K/S curve map of medium dyeing wool fiber, a in figure: conventional water-bath is dyeed; B:TX-100 reverse micelle dyes; C:TX-100/Span40 Mixed reverse micelles dyeing (1:2);
Fig. 3 is medium dyeing processes K/S curve map for reusing nonionic Mixed reverse micelles of the present invention;
Fig. 4 is medium dyeing wool fiber K/S curve map for reusing nonionic Mixed reverse micelles of the present invention.
Detailed description of the invention
Below in conjunction with drawings and Examples, the invention will be further described.
Nonionic Mixed reverse micelles in the present embodiment, comprises by mass percentage:
TX-100:2-12％，
Span：1-10％，
N-octyl alcohol: 10-35%,
Isooctane: 30-60%,
Dyestuff: 0.01-0.07%,
And distilled water: 0.1-6.0%.
Nonionic Mixed reverse micelles in the present embodiment, obtain its pool diameter through viscosimetry and be about 20-50nm, aggregation number is about 200-500, conductivity meter is adopted to obtain its electrical conductivity at 0-1.0 μ s/cm, its chemical stability is good, HLB value is lower, thus is conducive to dyestuff and dyes to fiber for medium with it.
And prior art reverse micelle particularly ion-type reverse micelle chemical stability is poor, and dyestuff is that the dyeability of medium to fiber is lower with it, and the HLB value of single non-ionic reverse micelle is higher, is unfavorable for that dyestuff dyes to fiber for medium with it.
Nonionic Mixed reverse micelles of the present invention comprises nonionic surface active agent TX-100 and Span because of its component, therefore can be described as again TX-100/Span Mixed reverse micelles.Compared with existing non-ionic reverse micelle, the design of reverse micelle of the present invention can not only by the Mixed reverse micelles system regulating the ratio of TX-100 and Span to obtain different key property, but also lower HLB value can be obtained, thus dyestuff with it for medium coloured fibre can obtain good dyeability.
In TX-100 reverse micelle, ACID DYES is to the dyeability of protein fibre than poor in conventional water-bath at present, and this may be owing to causing the competitive Adsorption of fiber between TX-100 and dyestuff, and this competition is relevant with the molecular weight of surfactant.Research shows, TX-100/Span Mixed reverse micelles of the present invention reduces the competi-tive acting force to fiber between surfactant and dyestuff, significantly improve the dyeability of ACID DYES to protein fibre, and compared with conventional water-bath decoration method, can carry out at low temperatures for medium staining for protein fiber with nonionic Mixed reverse micelles of the present invention, which significantly reduces dyeing cost.In addition, this Mixed reverse micelles is not only applicable to the dyeing of cellulose fibre and protein fibre, and all can use under acidity and weak base condition.
Dyestuff not only can obtain higher dyeability to cellulose fiber peacekeeping protein fibre in nonionic Mixed reverse micelles of the present invention, and Mixed reverse micelles of the present invention also has good repeat performance.With Mixed reverse micelles of the present invention for medium dyestuff almost overlaps to the cellulose fiber peacekeeping protein fibre stained specimens K/S curve obtained for five times that dyes, the total color difference within 0.5 (see Fig. 3 and Fig. 4 in Figure of description) of sample room.This shows that Mixed reverse micelles of the present invention still can make cellulose fiber peacekeeping protein fibre obtain good dyeability in reusing, and improve service efficiency significantly, its industrial applications has obvious economic benefit.
The preparation method of nonionic Mixed reverse micelles described in the present embodiment, comprises the following steps:
1) isooctane of certain mass, is taken at ambient temperature in dry beaker, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, in beaker, add TX-100, Span and the n-octyl alcohol of respective quality successively, finally use magnetic stirring apparatus to carry out rapid stirring to obtain flaxen mixing material to it;
2), aqueous dye solutions preparation: first take the ACID DYES of certain mass or REACTIVE DYES in the beaker of drying, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, the distilled water adding respective quality in beaker makes it to dissolve completely and obtains transparent aqueous dye solutions, regulate the pH value of aqueous dye solutions, with applicable reactive dyeing cellulose fibre or acid dyeing protein fibre;
3), then according to the mass ratio of composition each in nonionic Mixed reverse micelles, above-mentioned aqueous dye solutions implantation step 1 by respective volume) in preparation mixing material in obtain milky mixt, carry out ultrasonic wave process again after using magnetic stirring apparatus to stir milky mixt at ambient temperature, make it the nonionic Mixed reverse micelles system becoming transparence.
The preparation method of nonionic Mixed reverse micelles of the present invention and the maximum of prior art are not both and have employed TX-100 and Span two kinds of non-ionic surface active agents and prepare nonionic Mixed reverse micelles, the HLB value of mixed type reverse micelle is regulated by the consumption changing two kinds of surfactants, thus obtain the preferably fundamental characteristics such as electrical conductivity, pool diameter and aggregation number, significantly improving dyestuff with it is the dyeability of medium to textiles.Usually, adopt the protein fibres such as conventional water-bath dyeing wool to need to carry out under the hot conditions of 90 ~ 100 DEG C, which substantially increases the dyeing cost of textiles.Mixed reverse micelles preparation of the present invention and dyeing flow process are owing to carrying out at low temperatures, and thus technique is simple, and with low cost, do not need special installation, easily operate, industrialization promotion is easy.
In order to evaluate the dyeability of dyestuff to fiber in nonionic Mixed reverse micelles of the present invention, REACTIVE DYES and ACID DYES is adopted to dye to cellulose fiber peacekeeping protein fibre for medium with it below respectively, and be that the coloured fibre that medium obtains contrasts with the TX-100 reverse micelle of the conventional water-bath of employing and prior art, the place do not addressed in following technique is applicable to prior art.
(1) REACTIVE DYES is to the dyeing of cellulose fibre
1, REACTIVE DYES is adopted with nonionic Mixed reverse micelles of the present invention for medium dyes to cellulose fibre.
Before dyeing is carried out, first carry out preliminary treatment to cellulose fibre, its technique is:
In the aqueous solution containing 2.0g/L detergent, boil 10min by through concise, bleaching and the cellulose fibre of mercerization finish, then clean with cold water and dry in room temperature for subsequent use.
With nonionic Mixed reverse micelles for dyeing medium:
First by be placed in through pretreated about 1.0g cellulose fibre 50ml regulation dye strength by nonionic Mixed reverse micelles (because its component of nonionic Mixed reverse micelles of the present invention comprises nonionic surface active agent TX-100 and Span, therefore also can be described as TX-100/Span Mixed reverse micelles) as in the dyeing system of medium, then at 40-60 DEG C of temperature to textile dyeing 2-3 hour, then the sodium carbonate adding 5-10g/L carries out fixation to fabric, take out cellulose fibre after 0.5-1 hour to soap, and dry after fully washing, colour matching instrument and fastness instrument is finally adopted to measure case depth (K/S) curve and the fastness of dyeing cellulosic fibre.
To soap technique:
Working solution of soaping is the aqueous solution of soap powder containing 2g/L and 2g/L sodium carbonate.Bath raio is 1:30, and temperature of soaping is 95 DEG C, and the time of soaping is 10min.
2, REACTIVE DYES is adopted with the TX-100 reverse micelle of prior art for dyeing medium dyes to cellulose fibre.
The TX-100 reverse micelle adopting prior art is the technique that dyeing medium dyes to cellulose fibre, the dyeing in nonionic Mixed reverse micelles of itself and above-mentioned cellulose fibre is compared with technique of soaping, and unique difference is that whole dyeing course carries out in the TX-100 reverse micelle system of preparation.
3, REACTIVE DYES and conventional water-bath decoration method is adopted to dye to cellulose fibre.
First be placed in through pretreated about 1.0g cellulose fibre the aqueous dye solutions that 50ml specifies dye strength, start into dye at 55 DEG C, dye to add after 10 minutes 50% sodium chloride, the sodium chloride of 50% is added again after continuous dye 15 molecule, then the sodium carbonate adding normal concentration after dyeing again 15 minutes carries out fixation, fixation took out sample after 30 minutes, with cold water washing, soap boiling, washing and oven dry, colour matching instrument and fastness instrument is finally adopted to measure case depth (K/S) curve and the fastness of dyed cotton fabric.
(2) ACID DYES is to the dyeing of protein fibre
1, ACID DYES is adopted with nonionic Mixed reverse micelles of the present invention for medium dyes to protein fibre.
Before dyeing is carried out, first carry out preliminary treatment to protein fibre, its technique is:
The protein fibre of certain mass being placed in concentration is the 1.0g/L non-ionic surface active agent JFC aqueous solution, takes out after processing 30min under 40 DEG C and low rate mixing condition, and use distilled water repeatedly to rinse, then room temperature is dried for subsequent use.
With nonionic Mixed reverse micelles for dyeing medium:
First using be placed in respectively through pretreated about 1.0g protein fibre 50ml regulation dye strength by distilled water, TX-100 reverse micelle or the TX-100/Span Mixed reverse micelles dyeing system as medium, and adjust ph is to 1-3, then at 40-60 DEG C of temperature, protein fibre is dyeed 3 hours, the rear taking-up yarn that dyeed is soaped 10min under 60 DEG C and neutrallty condition, then it fully washed and dry, finally using colour matching instrument and fastness instrument to measure K/S curve and the fastness of staining for protein fiber respectively.
2, ACID DYES is adopted with the TX-100 reverse micelle of prior art for dyeing medium dyes to protein fibre.
The TX-100 reverse micelle adopting prior art is the technique that dyeing medium dyes to protein fibre, compare with technique of soaping with the dyeing of above-mentioned protein fibre in nonionic Mixed reverse micelles, unique difference is that whole dyeing course carries out in the TX-100 reverse micelle of preparation.
3, ACID DYES and conventional water-bath decoration method is adopted to dye to protein fibre.
First be placed in through pretreated about 1.0g protein fibre the aqueous dye solutions that 50ml specifies dye strength, then dye bath is made with the speed rapid temperature increases of 2 DEG C per minute to 100 DEG C, and 100 DEG C of dyeing 60 minutes, take out sample after dyeing, with cold wash, oven dry.
Wherein K/S1: the fiber sample dyeed for medium with TX-100/Span Mixed reverse micelles of the present invention is in the K/S value of maximum absorption wave strong point;
K/S2: the K/S value of fiber sample in maximum absorption wave strong point taking water as medium dyeing;
K/S3: the fiber sample dyeed for medium with prior art TX-100 reverse micelle is in the K/S value of maximum absorption wave strong point;
△ K/S1-2: the relatively conventional water-bath decoration method dyeing of the fiber sample obtained for medium dyes with Mixed reverse micelles of the present invention obtains the K/S value increment rate of stained specimens in maximum absorption wave strong point;
△K/S1-2＝(K/S1-K/S2)×100％/K/S2
△ K/S1-3: with Mixed reverse micelles of the present invention for medium dye the fiber obtained relative to the TX-100 reverse micelle of prior art for medium dyes the K/S value increment rate of the stained specimens obtained in maximum absorption wave strong point;
△K/S1-3＝(K/S1-K/S3)×100％/K/S3
(3) repeated using method of reverse micelle system:
First filtration treatment is carried out to remove fiber fragment wherein to reverse micelle raffinate after having dyeed, then ultraviolet-uisible spectrophotometer is adopted to measure the absorbance of reverse micelle raffinate, and use the dye strength in calibration curve method calculating reverse micelle raffinate, then in reverse micelle system, supplement aqueous dye solutions makes dye strength wherein reach the concentration value before dyeing, finally to be inserted by undyed fiber sample in reverse micelle system and to use identical dyeing to dye.
Compared with prior art, nonionic Mixed reverse micelles of the present invention can make fiber obtain better dyeability as medium, and under identical dye dosage condition, the K/S value of dyeing and fastness are apparently higher than the relevant parameter of traditional water bath dyeing.The more important thing is, nonionic Mixed reverse micelles system of the present invention has the advantage that chemical stability is high and reusing is good, dyeing water consumption can not only be reduced significantly, realize the low temperature dyeing of protein fibre, reach the target of energy-saving and emission-reduction, also can realize the salt-free dyeing of cellulose fibre, and preparation technology is simple, do not need special installation, easily operate, industrialization promotion has a bright future.
Introduce specific embodiments of the invention below, but the present invention is not by the restriction of embodiment, the place do not addressed in following examples method is applicable to prior art.
Embodiment 1: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the aqueous solution of reactive dye (pH=7) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:6.00%; Span:7.00%; N-octyl alcohol: 22.04%; Isooctane: 60.00%; Dyestuff: 0.01%; Distilled water: 4.95%, wherein dyestuff is to the heavy Owf=0.5% of fabric.
This reverse micelle is after measured: average diameter is 30nm; Aggregation number 300, electrical conductivity is at 0-0.2 μ s/cm.
This experiment for dyeing medium, adopts REACTIVE Red 195, Reactive Blue 222 and REACTIVE Yellow 145 three kinds of REACTIVE DYES at 60 DEG C to pure cotton woven fabric (100.7g/m with TX-100/Span40 reverse micelle respectively
2) carry out dyeing after 3 hours, then the sodium carbonate adding 8g/L carries out fixation to cotton fiber, take out cotton fiber after 1 hour to soap, and compare in the K/S value of maximum absorption wave strong point as the medium cotton fiber obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, result is as shown in table 1.
In addition, carry out fastness mensuration and grading with reference to standard GB/T/T 3921.1-1997 and GB/T 3920-1997 to stained specimens respectively, result is as table 2.
Table 1 adopts the different medium cotton fiber K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| REACTIVE Red 195 | 6.44 | 3.35 | 5.43 | 92％ | 19％ |
| Reactive Blue 222 | 6.48 | 4.02 | 4.77 | 56％ | 32％ |
| REACTIVE Yellow 145 | 5.85 | 3.50 | 4.42 | 67％ | 32％ |
The different medium that adopts table 2 dyes the cotton fiber fastness evaluation obtained
Embodiment 2: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the aqueous solution of reactive dye (pH=7) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:12.00%; Span:10.00%; N-octyl alcohol: 23.02%; Isooctane: 50.00%; Dyestuff: 0.03%; Distilled water: 4.95%, wherein dyestuff is to the heavy Owf=1.0% of fabric.
This reverse micelle is after measured: average diameter is 30nm; Aggregation number 300, electrical conductivity is at 0-0.2 μ s/cm.
This experiment for dyeing medium, adopts REACTIVE Red 195, Reactive Blue 222 and REACTIVE Yellow 145 three kinds of REACTIVE DYES at 60 DEG C to pure cotton woven fabric (100.7g/m with TX-100/Span40 reverse micelle respectively
2) carry out dyeing after 3 hours, then the sodium carbonate adding 9g/L carries out fixation to cotton fiber, take out cotton fiber after 1 hour to soap, and compare in the K/S value of maximum absorption wave strong point as the medium cotton fiber obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, result is as shown in table 3.
In addition, carry out fastness mensuration and grading with reference to standard GB/T/T3921.1-1997 and GB/T3920-1997 to stained specimens respectively, result is as table 4.
Table 3 adopts the different medium cotton fiber K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| REACTIVE Red 195 | 13.23 | 6.72 | 10.96 | 97％ | 21％ |
| Reactive Blue 222 | 12.47 | 7.73 | 10.01 | 61％ | 25％ |
| REACTIVE Yellow 145 | 12.16 | 7.02 | 9.89 | 73％ | 23％ |
The different medium that adopts table 4 dyes the cotton fiber fastness evaluation obtained
Embodiment 3: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the aqueous solution of reactive dye (pH=7) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:8.00%; Span:5.00%; N-octyl alcohol: 27.00%; Isooctane: 55.00%; Dyestuff: 0.05%; Distilled water: 4.95%, wherein dyestuff is to the heavy Owf=2.0% of fabric.
This reverse micelle is after measured: average diameter is 30nm; Aggregation number 300, electrical conductivity is at 0-0.2 μ s/cm.
Adopt REACTIVE Red 195, Reactive Blue 222 and REACTIVE Yellow 145 three kinds of REACTIVE DYES respectively at 60 DEG C to pure cotton woven fabric (100.7g/m
2) carry out dyeing after 3 hours, then the sodium carbonate adding 10g/L carries out fixation to cotton fiber, take out cotton fiber after 1 hour to soap, and compare in the K/S value of maximum absorption wave strong point as the medium cotton fiber obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, result is as shown in table 5.
In addition, carry out fastness mensuration and grading with reference to standard GB/T/T3921.1-1997 and GB/T3920-1997 to stained specimens respectively, result is as table 6.
Table 5 adopts the different medium cotton fiber K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| REACTIVE Red 195 | 19.53 | 11.89 | 17.34 | 64％ | 13％ |
| Reactive Blue 222 | 18.48 | 14.25 | 16.15 | 30％ | 14％ |
| REACTIVE Yellow 145 | 16.75 | 13.50 | 13.85 | 24％ | 21％ |
The different medium that adopts table 6 dyes the cotton fiber fastness evaluation obtained
Embodiment 4: this example is Contrast on effect example.Take REACTIVE Red 195 as research object, different Span and TX-100 is adopted to be mixed with different nonionic Mixed reverse micelles according to the technique of embodiment 3, and respectively with its for medium adopt REACTIVE Red 195 pure cotton woven fabric is dyeed, wherein Span is respectively Span80, Span60 and Span40, and dyestuff is to the heavy Owf=2.0% of fabric.To the stained specimens obtained using this Mixed reverse micelles as medium and conventional water-bath decoration method and prior art TX-100 reverse micelle for the medium cotton fiber obtained that dyes measures in the K/S value of maximum absorption wave strong point and compares, and evaluate the fastness of each stained specimens, result is as table 7-8.
Table 7 adopts different Mixed reverse micelles to be that the medium cotton fiber K/S value obtained that dyes compares
| Span type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| TX-100/Span80 | 19.09 | 11.89 | 17.34 | 61％ | 10％ |
| TX-100/Span60 | 19.21 | 11.89 | 17.34 | 62％ | 11％ |
| TX-100/Span40 | 19.53 | 11.89 | 17.34 | 64％ | 13％ |
Table 8 adopts different Mixed reverse micelles to be that medium dyes the cotton fiber fastness evaluation obtained
Embodiment 5: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the ACID DYES aqueous solution (pH=1) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:6.00%; Span:8.00%; N-octyl alcohol: 23.99%; Isooctane: 56%; Dyestuff: 0.01%; Distilled water: 6.0%, wherein dyestuff is to the heavy Owf=0.5% of fabric.
This reverse micelle is after measured: average diameter is 20nm; Aggregation number 200, electrical conductivity is at 0.2-1 μ s/cm.
This experiment for dyeing medium, adopts ACID BLACK 234, Acid Red G and acid light yellow three kinds of ACID DYES at 60 DEG C to wool fibre (223.6g/m with TX-100/Span40 Mixed reverse micelles respectively
2) dye, and compare in the K/S value of maximum absorption wave strong point as the medium wool fibre obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, finally measure the fastness of each stained specimens, result is as table 9-10.
Table 9 adopts the different medium wool fibre K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| ACID BLACK 234 | 7.33 | 5.27 | 4.31 | 39％ | 70％ |
| Acid Red G | 14.95 | 11.8 | 9.09 | 27％ | 64％ |
| Acid light yellow | 11.78 | 9.66 | 7.21 | 22％ | 63％ |
The different medium that adopts table 10 dyes the wool fibre fastness evaluation obtained
Embodiment 6: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the ACID DYES aqueous solution (pH=1) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:9.00%; Span:7.00%; N-octyl alcohol: 29.83%; Isooctane: 54%; Dyestuff: 0.07%; Distilled water: 0.1%, wherein dyestuff is to the heavy Owf=1.0% of fabric.
This reverse micelle is after measured: average diameter is 20nm; Aggregation number 200, electrical conductivity is at 0.2-1 μ s/cm.
This experiment with TX-100/Span40 Mixed reverse micelles for dyeing medium, ACID BLACK 234, Acid Red G and acid light yellow three kinds of ACID DYES are adopted to dye to wool fibre at 60 DEG C respectively, and compare in the K/S value of maximum absorption wave strong point as the medium wool fibre obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, and measuring the fastness of each stained specimens, result is as table 11-12.
Table 11 adopts the different medium wool fibre K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| ACID BLACK 234 | 11.20 | 8.33 | 7.94 | 34％ | 41％ |
| Acid Red G | 29.69 | 23.98 | 21.76 | 24％ | 36％ |
| Acid light yellow | 19.99 | 17.39 | 15.29 | 15％ | 31％ |
The different medium that adopts table 12 dyes the wool fibre fastness evaluation obtained
Embodiment 7: first accurately take the isooctane of certain mass at ambient temperature in dry beaker, then add TX-100, Span40 of prescribed volume and n-octyl alcohol successively in beaker, and use magnetic stirring apparatus to stir to obtain flaxen mixing material to it.Then use microsyringe that the ACID DYES aqueous solution (pH=1) of prescribed volume is injected mixed solution, and use magnetic stirring apparatus to stir it at ambient temperature, carry out ultrasonic wave process again after about 10min, finally obtain the TX-100/Span40 nonionic Mixed reverse micelles system of transparence.Wherein, the mass percent that each component accounts for whole reverse micelle system is respectively: TX-100:2%; Span:1%; N-octyl alcohol: 35%; Isooctane: 60%; Dyestuff: 0.07%; Distilled water: 1.93%, wherein dyestuff is to the heavy Owf=2.0% of fabric.
This reverse micelle is after measured: average diameter is 20nm; Aggregation number 200, electrical conductivity is at 0.2-1 μ s/cm.
This experiment with TX-100/Span40 Mixed reverse micelles for dyeing medium, ACID BLACK 234, Acid Red G and acid light yellow three kinds of ACID DYES are adopted to dye to wool fibre at 60 DEG C respectively, and compare in the K/S value of maximum absorption wave strong point as the medium wool fibre obtained that dyes with conventional water-bath decoration method and prior art TX-100 reverse micelle, and measuring the fastness of each stained specimens, result is as table 13-14.
Table 13 adopts the different medium wool fibre K/S value obtained that dyes to compare
| Dye type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| ACID BLACK 234 | 16.91 | 14.22 | 13.88 | 19％ | 22％ |
| Acid Red G | 37.95 | 34.44 | 31.14 | 10％ | 22％ |
| Acid light yellow | 25.23 | 23.60 | 21.58 | 7％ | 17％ |
The different medium that adopts table 14 dyes the wool fibre fastness evaluation obtained
Embodiment 8: this example is Contrast on effect example.Take ACID BLACK 234 as research object, adopt different Span and TX-100 to prepare different nonionic Mixed reverse micelles according to the technique of embodiment 6, and respectively with its for medium adopt ACID BLACK 234 wool fibre is dyeed.Wherein Span adopts Span80, Span60 and Span40 respectively, and dyestuff is to the heavy Owf=2.0% of fabric.Be that the medium wool fibre obtained that dyes measures in the K/S value of maximum absorption wave strong point and compares to the stained specimens obtained and conventional water-bath decoration method and prior art TX-100 reverse micelle, and evaluate the fastness of each stained specimens, result is as table 15-16.
Table 15 adopts different Mixed reverse micelles to be that the medium wool fibre K/S value obtained that dyes compares
| Span type | K/S 1 | K/S 2 | K/S 3 | △K/S 1-2 | △K/S 1-3 |
| Span80 | 15.50 | 14.22 | 13.88 | 9％ | 12％ |
| Span60 | 16.60 | 14.22 | 13.88 | 17％ | 20％ |
| Span40 | 16.91 | 14.22 | 13.88 | 19％ | 22％ |
Table 16 adopts different Mixed reverse micelles to be that medium dyes the wool fibre fastness evaluation obtained
Can see from table 1-6 and table 9-14, nonionic phenotype reverse micelle of the present invention is adopted to be that dyeing medium dyes to cotton fiber and wool fibre respectively, the stained specimens obtained is all the coloured fibre K/S value that medium obtains higher than the TX-100 reverse micelle of conventional water-bath decoration method and prior art in the K/S value of maximum absorption wave strong point, and stained specimens has good fastness to rubbing and color fastness to washing, all more than 4 grades.This explanation significantly can improve the dyeability of dyestuff to fiber using nonionic Mixed reverse micelles of the present invention as dyeing medium, and does not significantly affect the dyefastness of fiber.
Table 7-8 and table 15-16 display, Span80, Span60 and Span40 all can form nonionic Mixed reverse micelles with TX-100, and dyestuff using it as dyeing medium to the dyeability of fiber all higher than the TX-100 reverse micelle of conventional water-bath decoration method and prior art for medium is to the dyeability of fiber, the fastness of coloured fibre, all more than 4 grades, has good fastness to rubbing and color fastness to washing.
Fig. 1 and Fig. 2 shows, dyestuff to dye the stained specimens obtained using nonionic Mixed reverse micelles as medium to cotton fiber and wool fibre, the TX-100 reverse micelle of its K/S curve shape and conventional water-bath decoration method and prior art is that the dye stained specimens that obtains of medium is identical, and the maximum absorption wavelength of stained specimens does not all change yet, this illustrates that the fiber dyeing method using nonionic Mixed reverse micelles of the present invention as dyeing medium is feasible, and stained specimens is that medium dyes the fiber sample obtained at the TX-100 reverse micelle that the K/S value that maximum absorption wave strong point obtains all is greater than conventional water-bath dyeing and prior art, illustrate that dyestuff carries out dyeing using nonionic Mixed reverse micelles of the present invention as dyeing medium to fiber and can obtain better dyeability.In addition, can see from Fig. 3 and Fig. 4, reuse the stained specimens that nonionic Mixed reverse micelles of the present invention obtains for five times stock-dye as dyestuff during dyeing medium, its K/S curve almost overlaps, and this also shows that nonionic Mixed reverse micelles can be good at recycling in the tint applications of fiber as dyeing medium.
The present invention, as a kind of clean dyeing and finishing processing method of energy-saving and water-saving, compared with conventional coloring method, the method significantly reduces the existence of water in the middle of dyeing process, decrease the pollution of water, and can repetitive cycling use, can carry out at low temperatures, this greatly reduces printing and dyeing cost.With its saving at the energy, the protection of environment, the advantage of the aspects such as the saving of water and the clean and safe of working environment, will have broad prospects.
What finally illustrate is, above embodiment is only in order to illustrate technical scheme of the present invention and unrestricted, although with reference to preferred embodiment to invention has been detailed description, those of ordinary skill in the art is to be understood that, can modify to technical scheme of the present invention or equivalent replacement, and not departing from aim and the scope of technical solution of the present invention, it all should be encompassed in the middle of right of the present invention.
Claims (2)
1. a nonionic Mixed reverse micelles, is characterized in that: comprise by mass percentage:
TX-100:2-12％，
Span：1-10％，
N-octyl alcohol: 10-35%,
Isooctane: 30-60%,
Dyestuff: 0.01-0.07%,
And distilled water: 0.1-6.0%.
2. a preparation method for nonionic Mixed reverse micelles described in claims 1, is characterized in that: comprise the following steps:
1) isooctane of certain mass, is taken at ambient temperature in dry beaker, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, in beaker, add TX-100, Span and the n-octyl alcohol of respective quality successively, finally use magnetic stirring apparatus to carry out rapid stirring to obtain flaxen mixing material to it;
2), aqueous dye solutions preparation: first take the ACID DYES of certain mass or REACTIVE DYES in the beaker of drying, then according to the mass ratio of composition each in nonionic Mixed reverse micelles, the distilled water adding respective quality in beaker makes it to dissolve completely and obtains transparent aqueous dye solutions, regulate the pH value of aqueous dye solutions, with applicable reactive dyeing cellulose fibre or acid dyeing protein fibre;
3), then according to the mass ratio of composition each in nonionic Mixed reverse micelles, above-mentioned aqueous dye solutions implantation step 1 by respective volume) in preparation mixing material in obtain milky mixt, carry out ultrasonic wave process again after using magnetic stirring apparatus to stir milky mixt at ambient temperature, make it the nonionic Mixed reverse micelles system becoming transparence.
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