CN111424446A - Supercritical dyeing method - Google Patents
Supercritical dyeing method Download PDFInfo
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- CN111424446A CN111424446A CN202010434606.1A CN202010434606A CN111424446A CN 111424446 A CN111424446 A CN 111424446A CN 202010434606 A CN202010434606 A CN 202010434606A CN 111424446 A CN111424446 A CN 111424446A
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- dyeing
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/94—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dyes dissolved in solvents which are in the supercritical state
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/16—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using dispersed, e.g. acetate, dyestuffs
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/38—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using reactive dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P1/00—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed
- D06P1/44—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders
- D06P1/60—General processes of dyeing or printing textiles, or general processes of dyeing leather, furs, or solid macromolecular substances in any form, classified according to the dyes, pigments, or auxiliary substances employed using insoluble pigments or auxiliary substances, e.g. binders using compositions containing polyethers
- D06P1/613—Polyethers without nitrogen
- D06P1/6131—Addition products of hydroxyl groups-containing compounds with oxiranes
- D06P1/6133—Addition products of hydroxyl groups-containing compounds with oxiranes from araliphatic or aliphatic alcohols
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/6033—Natural or regenerated cellulose using dispersed dyes
-
- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06P—DYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
- D06P3/00—Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
- D06P3/58—Material containing hydroxyl groups
- D06P3/60—Natural or regenerated cellulose
- D06P3/66—Natural or regenerated cellulose using reactive dyes
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Coloring (AREA)
Abstract
Disclosed is a dyeing method comprising: placing natural fiber fabric, reactive disperse dye, fatty alcohol-polyoxyethylene ether, triethylene diamine, ethanol and carbon dioxide fluid into a dyeing device; fully stirring and standing; pressurizing to a certain pressure and heating to a certain temperature; dyeing under the conditions of heat preservation and pressure maintaining. The dyeing method can form reverse micelles, and can improve the dyeing performance of natural fibers, particularly cotton fiber fabrics.
Description
Technical Field
The invention belongs to the technical field of dyeing; relates to a supercritical dyeing technology; and more particularly, to a dyeing method for supercritical carbon dioxide anhydrous dyeing.
Background
Water is an essential and important resource for human survival. Although the water resource on the earth is abundant, the fresh water available for human on land only accounts for 2.5% of the total fresh water resource. The water resource of China is more deficient, and the occupied amount per person is only one fourth of the average level in the world; furthermore, the fresh water resources are not distributed uniformly, and a plurality of areas such as the north and the northwest are seriously lack of water. Meanwhile, the current situations of water environment deterioration, water quality type water shortage and water resource shortage are increasingly aggravated. In order to change the current situation, the public environment protection awareness of society is continuously strengthened, and the country also develops a plurality of laws and regulations related to environment protection. In recent years, environmental storms scrapped against various pollution industries have also become more severe. As the textile printing and dyeing industry with huge water resource consumption and serious pollution, the development of water-saving and even waterless dyeing or printing process with high process efficiency is becoming more and more concerned.
Research shows that the traditional dyeing method consumes a great deal of water. The water amount of 100-200 tons is required for printing and dyeing 1 ton of textiles on average. Although a small part of water can be recycled, the rest is mostly waste water. Therefore, the waste water discharged by the printing and dyeing industry also becomes a main source of the whole textile industry, and accounts for almost more than 80%. Furthermore, in conventional dyeing processes, various dyeing auxiliaries are usually added to the dyebath. The dyeing auxiliary agents and unfixed dye remain in the printing and dyeing wastewater, thus increasing the burden of later-stage sewage treatment and bringing serious threat to the ecological environment.
As a novel, green and environment-friendly printing and dyeing technology, the supercritical carbon dioxide fluid anhydrous dyeing technology injects vitality for innovation of the textile industry, and meanwhile, the technology can really realize ecological spinning, accords with the concepts of energy conservation, emission reduction and sustainable development, and has positive practical significance.
The supercritical carbon dioxide fluid not only has the properties of low viscosity and strong diffusion of gas, but also has the density similar to that of liquid and has good dissolving capacity for hydrophobic substances. The above-mentioned advantageous properties of carbon dioxide fluid are utilized as a dyeing medium to replace the water of a conventional dye bath for dyeing textiles. The supercritical carbon dioxide dyeing does not need water in the whole dyeing process, and dyeing liquor does not need adding dyeing auxiliary agents, acid, alkali and other chemical reagents. The dyed fabric does not need to be washed in a floating color, and the generation of dyeing wastewater is avoided, so that the treatment problem of dyeing wastewater is really solved at the source, and the method is beneficial to environmental protection. In addition, the dyed fabric is in a dry state, and does not need to be dried, thereby being beneficial to saving energy. The residual dye and carbon dioxide fluid can be continuously used in the next dyeing process.
Since carbon dioxide is a nonpolar molecule, according to the principle of similar phase solubility, a nonpolar or low-polarity dye has good solubility in a supercritical carbon dioxide fluid, and thus, the dye for dyeing with supercritical carbon dioxide is mainly a disperse dye. Accordingly, as dyed fabrics, the most widely used and successful are primarily polyester fabrics, followed by aramid and polypropylene fabrics. In the textile market, however, natural fiber fabrics, especially cotton fabrics, generally hold a large share and are highly appreciated by consumers due to their natural material origin and the additional green attributes. However, such fibers are usually dyed using reactive dyes and acid dyes, which are easily soluble in water but not in carbon dioxide fluid, and thus have technical bottlenecks in applying supercritical carbon dioxide fluid dyeing technology.
In recent years, the problem of dyeing natural fibers in supercritical carbon dioxide fluid has been mainly addressed from the following points. The method specifically comprises the following steps:
the natural fiber is pretreated by the swelling agent or the cross-linking agent, so that the number of hydrogen bonds on the surface of the natural fiber is reduced, and the polarity of the natural fiber is reduced.
The addition of a polar co-solvent (primarily water and ethanol) to the carbon dioxide fluid increases the polarity of the carbon dioxide fluid, thereby improving the solubility of the dye in the carbon dioxide fluid.
Under the premise of basically not changing the polarity of the original dye, active groups are introduced into the disperse dye molecules, and the formed active disperse dye has the advantages of good solubility and strong reactivity of the disperse dye and reacts with natural fibers through nucleophilic addition or substitution reaction. However, most reactive disperse dyes still have the disadvantage of not being very reactive with natural fibers, especially cotton fibers.
The surfactant is added into the carbon dioxide fluid to form reverse micelles, so that the solubility of the dye can be improved; meanwhile, the hydrolysis degree of the dye is inhibited, and the reactivity of the dye can be improved to a certain degree.
Chinese patent application CN105696384A discloses a reverse micelle supercritical CO of polyester-cotton blended fabric2The dyeing system comprises the following components in parts by weight: 5-25 parts of penta-polyethylene glycol mono-octyl ether, n-amyl alcohol: 10-35 parts of reactive dye: 0.01-0.20 parts of disperse dye: 0.01-0.10 parts of carbon dioxide: 40-60 parts of distilled water: 0.01E6.0 parts. Placing the polyester-cotton blended fabric in a high-pressure container, and then carrying out reverse micelle supercritical CO2The dyeing system has good solubility, disperse dye is simultaneously dyed on the polyester fiber while the active dye is used for dyeing the cotton fiber components, and the cotton fiber is dyed under the salt-free condition, so that the phenomena of staining and stain of the dye on the fabric are greatly avoided; meanwhile, the dyeing method has the advantages of high dyeing efficiency, excellent dyeing effect and the like.
However, the above patent application does not disclose specific reactive dyes and disperse dyes, resulting in difficult reproducibility of dyeing properties of the dyeing system.
Therefore, there is still a need to provide a dyeing method for anhydrous dyeing of natural fibers, especially cotton fabrics, with supercritical carbon dioxide.
Disclosure of Invention
The invention aims to provide a dyeing method for supercritical carbon dioxide anhydrous dyeing. The dyeing method not only enables the dyeing composition to have better solubility in supercritical carbon dioxide, but also enables the dyed natural fiber fabrics, especially cotton fabrics, to have excellent dyeing performance.
In order to solve the technical problems, the invention adopts the following technical scheme: a method of dyeing comprising:
placing natural fiber fabric, reactive disperse dye, fatty alcohol-polyoxyethylene ether, triethylene diamine, ethanol and carbon dioxide fluid into a dyeing device; fully stirring and standing; pressurizing to a certain pressure and heating to a certain temperature; dyeing under the conditions of heat preservation and pressure maintaining; it is characterized in that the molecular formula of the fatty alcohol-polyoxyethylene ether is R- (OCH)2CH2)n-OH; r is selected from C16-18A fatty alcohol residue; n is 10.
In the invention, the fatty alcohol-polyoxyethylene ether is selected from cetearyl alcohol-polyoxyethylene ether-10.
The dyeing method is characterized in that the natural fiber fabric is selected from cotton fabrics.
The dyeing method provided by the invention is characterized in that the bath ratio of the natural fiber fabric to the carbon dioxide fluid is 1 (400-600) (g/ml).
Preferably, the bath ratio of the cotton fabric to the carbon dioxide fluid is 1 (420-; more preferably, the bath ratio of the cotton fabric to the carbon dioxide fluid is 1 (450-550) (g/ml); and the bath ratio of the cotton fabric to the carbon dioxide fluid is 1 (480-520) (g/ml).
In a specific embodiment, the bath ratio of the cotton fabric to the carbon dioxide fluid is 1:500 (g/ml).
The dyeing method according to the invention, wherein the reactive disperse dye is selected from compounds of formula (I-1),
the dyeing method of the invention is characterized in that the amount of the reactive disperse dye is 0.25-4 omf%.
Preferably, the amount of the active disperse dye is 0.5-3.5 omf%; more preferably, the amount of the reactive disperse dye is 1.0-3 omf%; and, most preferably, the reactive disperse dye is used in an amount of 1.5 to 2.5 omf%.
In a specific embodiment, the reactive disperse dye is used in an amount of 2 omf%.
The dyeing method provided by the invention is characterized in that the dosage of the fatty alcohol-polyoxyethylene ether is 0.5-1.5 g/L calculated based on the volume of the carbon dioxide fluid.
Preferably, the fatty alcohol-polyoxyethylene ether is present in an amount of 0.6-1.4 g/L, based on the volume of the carbon dioxide fluid, more preferably, the fatty alcohol-polyoxyethylene ether is present in an amount of 0.7-1.2 g/L, based on the volume of the carbon dioxide fluid, and, most preferably, the fatty alcohol-polyoxyethylene ether is present in an amount of 0.8-1.0 g/L, based on the volume of the carbon dioxide fluid.
In one embodiment, the fatty alcohol-polyoxyethylene ether is used in an amount of 0.9 g/L, based on the volume of the carbon dioxide fluid.
The dyeing method comprises the step of using triethylene diamine and the active disperse dye in an amount of (2.6-5.8):1 (w/w).
Preferably, the amount of the triethylene diamine and the reactive disperse dye is (3-5.4):1 (w/w); more preferably, the amount of triethylene diamine and the active disperse dye is (3.4-5):1 (w/w); and, most preferably, triethylene diamine and the reactive disperse dye are used in an amount of (3.8-4.6):1 (w/w).
In a specific embodiment, triethylene diamine is used in an amount of 4.2:1(w/w) with the reactive disperse dye.
The dyeing method according to the invention, wherein the amount of ethanol is 0.5-5 g/L, calculated on the volume of the carbon dioxide fluid.
Preferably, the amount of ethanol is 1-4/L, based on the volume of the carbon dioxide fluid, more preferably, the amount of ethanol is 1.5-3.5 g/L, based on the volume of the carbon dioxide fluid, and, most preferably, the amount of ethanol is 2-3 g/L, based on the volume of the carbon dioxide fluid.
In one embodiment, the amount of ethanol used is 2.5 g/L, based on the volume of the carbon dioxide fluid.
The dyeing method of the invention is characterized in that the pressure is 18-32 MPa.
Preferably, the pressure is 20-30 MPa; more preferably, the pressure is 22-28 MPa; and, most preferably, the pressure is 24-26 MPa.
In a specific embodiment, the pressure is 25 MPa.
The dyeing method of the invention, wherein the temperature is 110-150 ℃.
Preferably, the temperature is 115-145 ℃; more preferably, the temperature is 120-140 ℃; and, most preferably, the temperature is 125-.
In a specific embodiment, the temperature is 130 ℃.
The dyeing method provided by the invention is characterized in that the dyeing time is 30-150 min.
Preferably, the dyeing time is 45-120 min; more preferably, the dyeing time is 50-90 min; and, most preferably, the staining time is 55-75 min.
In a specific embodiment, the temperature is 60 min.
The inventor finds that the dyeing method not only enables the dyeing composition to have better solubility in supercritical carbon dioxide, but also enables the dyeing composition to have excellent dyeing performance when used for dyeing natural fiber fabrics, particularly cotton fabrics.
Without wishing to be bound by any theory, the staining process described in the present invention is capable of forming reverse micelles. In the micelle, the supercritical carbon dioxide fluid forms an 'oil phase', the lipophilic end of the surfactant is deeply inserted into the supercritical carbon dioxide fluid, and the hydrophilic end spontaneously aggregates into a spherical micelle, so that a microemulsion with stable thermodynamic properties and containing a polar inner core is formed in the micelle; and the reactive disperse dye and the triethylene diamine are dissolved in a cosolvent to form a water-like phase. This is very advantageous for improving the solubility of the reactive disperse dyes in supercritical carbon dioxide and also for improving the dyeing properties of natural fibers, especially cotton fabrics.
Detailed Description
The invention will be further illustrated with reference to specific embodiments.
It should be understood that the detailed description of the invention is merely illustrative of the spirit and principles of the invention and is not intended to limit the scope of the invention. Furthermore, it should be understood that various changes, substitutions, deletions, modifications or adjustments may be made by those skilled in the art after reading the disclosure of the present invention, and such equivalents are also within the scope of the invention as defined in the appended claims.
In the invention, the technical indexes for evaluating the dyeing performance are soaping color fastness and rubbing color fastness which are respectively evaluated according to GB/T3921-.
Example 1
The composition for supercritical carbon dioxide anhydrous dyeing is prepared, and comprises reactive disperse dye, carbon dioxide fluid, fatty alcohol-polyoxyethylene ether, ethanol and triethylene diamine, wherein the reactive disperse dye is selected from the reactive disperse dye (a compound shown in a formula (I-1)) and is used in an amount of 2 omf%, the fatty alcohol-polyoxyethylene ether is selected from cetearyl alcohol-polyoxyethylene ether-10 and is used in an amount of 0.9 g/L calculated based on the volume of the carbon dioxide fluid, the ethanol is used in an amount of 2.5 g/L calculated based on the volume of the carbon dioxide fluid, and the triethylene diamine and the reactive disperse dye are used in an amount of 4.2:1 (w/w).
Converting according to the ratio of 1:500(g/ml) of carbon dioxide fluid bath, and fixing the cotton fabric with corresponding weight on a dyeing warp beam; then dissolving the reactive disperse dye, the surfactant and the triethylene diamine in the formula ratio in the cosolvent, and adding the cosolvent into a dyeing kettle. And then pumping carbon dioxide fluid into the dyeing kettle, sealing the dyeing kettle, fully stirring and standing for 1h (in the process, the carbon dioxide fluid and the surfactant form a reverse micelle system). The pressurizing and heating apparatus was further started until the pressure was 25MPa and the temperature was 130 ℃. Then dyeing is carried out for 60min under the condition of heat preservation and pressure maintaining. After dyeing is finished, releasing pressure and separating residual active disperse dye and carbon dioxide fluid through a separation kettle; and finally taking out the dyed cotton fabric.
Comparative example 1
The other conditions were the same as in example 1, except that no surfactant was added.
Evaluation of dyeing Properties
The soaping fastness and rubbing fastness of the dyed cotton fabrics of example 1 and comparative example 1 were determined as described previously. The results are shown in Table 1.
TABLE 1
As can be seen from Table 1, the dyed cotton fabric of example 1 according to the invention has significantly higher fastness to soaping and rubbing than comparative example 1.
The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention, and various modifications and changes may be made by those skilled in the art. Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention shall fall within the protection scope of the present invention.
Claims (10)
1. A method of dyeing comprising:
placing natural fiber fabric, reactive disperse dye, fatty alcohol-polyoxyethylene ether, triethylene diamine, ethanol and carbon dioxide fluid into a dyeing device; fully stirring and standing; pressurizing to a certain pressure and heating to a certain temperature; dyeing under the conditions of heat preservation and pressure maintaining; it is characterized in that the molecular formula of the fatty alcohol-polyoxyethylene ether is R- (OCH)2CH2)n-OH; r is selected from C16-18A fatty alcohol residue; n = 10.
2. The dyeing method according to claim 1, wherein the bath ratio of the natural fiber fabric to the carbon dioxide fluid is 1 (400-600) (g/ml).
3. The dyeing method according to claim 1, wherein the reactive disperse dye is selected from compounds of formula (I-1),
4. The dyeing method according to claim 1, wherein the reactive disperse dye is used in an amount of 0.25-4 omf%.
5. Dyeing process according to claim 1, in which the fatty alcohol-polyoxyethylene ether is used in an amount of 0.5 to 1.5 g/L, calculated on the volume of the carbon dioxide fluid.
6. The dyeing method according to claim 1, wherein the amount of triethylenediamine to the reactive disperse dye is (2.6-5.8):1 (w/w).
7. Dyeing process according to claim 1, in which the amount of ethanol used is between 0.5 and 5 g/L, calculated on the volume of carbon dioxide fluid.
8. Dyeing process according to claim 1, in which the pressure is between 18 and 32 MPa.
9. The method of claim 1, wherein the temperature is 110-150 ℃.
10. The dyeing method according to claim 1, wherein the dyeing time is 30 to 150 min.
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| CN202010434606.1A CN111424446A (en) | 2020-05-21 | 2020-05-21 | Supercritical dyeing method |
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