CN103614930A - Anhydrous recycling dyeing method of activated dye - Google Patents
Anhydrous recycling dyeing method of activated dye Download PDFInfo
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Abstract
The invention relates to an anhydrous recycling dyeing method of an activated dye. The method comprises the following steps: adding the dye to a polar organic solvent; adding electrolyte and organic alkali, and dissolving, so as to obtain a dye bath, wherein the proportional relation of the dye to the polar organic solvent to the electrolyte to the organic alkali is (0.5-30g):1L:(0-10g):(0.1-30g); pre-swelling a pure cotton fabric in the polar organic solvent at 50-150 DEG C for 0.5-24 hours; then dyeing in the dye bath at 45-130 DEG C for 0.5-3 hours at the dyeing bath ratio of 1:10 to 1:50; and cleaning and drying, so as to obtain the dyed fabric. The residual dye liquid generated in the method disclosed by the invention does not contain a hydrolyzed dye, and can achieve recycling of dye liquor just by directly supplying the dye and assistants.
Description
Technical field
The invention belongs to fabric dyeing method field, particularly the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES.
Background technology
REACTIVE DYES emerged so far from 1956, developed rapidly because chromatogram is complete, bright-colored, easy to use, had become the main dyestuff of cellulose dyeing.Along with the sternness increasingly of ecological environment problem, the caused problem of reactive dyeing is further outstanding.In reactive dyeing waste liquid, contain a large amount of inorganic salts that add up to hydrolised dye and the REACTIVE DYES of 30%-40% in water dyeing, all increased waste water treatment difficulty.
In non-aqueous system, dye, be considered to greatly to reduce the environmental protection staining technique of the non-water discharge of printing and dyeing.This type of studies multiplex critical carbon dioxide or weak level property halogenated hydrocarbon solvent as dyeing medium.Due to these media and larger cellulose fibre and the REACTIVE DYES compatibility of polarity poor, poor effect often aspect cellulose dyeing, need in system, introduce a small amount of water carries out swelling and promotes to dye the dissolving (CHAVAN of material cellulose fibre, R.B.and A.SUBRAMANIAN, dyeing cotton with a reactive dye from polar-nonpolar solvent systems.Textile Research Journal, 1983.53:p.539; Sawada, K.and M.Ueda, Adsorption and fixation of a reactive dye on cotton in non ?aqueous systems.Coloration technology, 2003.119 (3): p.182-186.).Such system not proper " anhydrous ", can not avoid the hydrolysis of dyestuff completely.
Summary of the invention
Technical problem to be solved by this invention is to provide the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES, and the method realizes the dyeing of non-water, avoids the problem that REACTIVE DYES cannot fixation because of hydrolysis in dyeing course.
The anhydrous colouring method capable of circulation of a kind of REACTIVE DYES of the present invention, comprising:
(1) dyestuff is added in polar organic solvent, then add electrolyte, organic base, ultrasonic or heating for dissolving, obtain dye bath; Wherein the proportionate relationship of dyestuff, polar organic solvent, electrolyte, organic base is 0.5-30g:1L:0-10g:0.1-30g;
(2) by pure cotton fabric in polar organic solvent, under 50 ℃ of-150 ℃ of conditions, pre-swelling 0.5-24h, then in above-mentioned dye bath, dye, dye bath ratio is 1:10-1:50, and dyeing temperature is 45-130 ℃, dyeing time is 0.5-3h, clean, be dried, obtain DYED FABRICS, wherein the proportionate relationship 6-7g:300ml of pure cotton fabric and polar organic solvent.
In described step (1), dyestuff is s-triazine, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) or halogen pyrimidines REACTIVE DYES.
Dyestuff is a kind of in CI active red, CI reactive black, CI active red, CI reactive orange in described step (1).
Electrolyte in described step (1) is for having the organic or inorganic alkali metal salt of certain solubility at dyeing solvent.
In described step (1), electrolyte is one or more in KI, sodium iodide, potassium bromide, sodium bromide, potassium nitrate, sodium nitrate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid potassium, sodium tetrafluoroborate, sodium hexafluoro phosphate.
Described electrolyte promotes dyestuff to absorb.
In described step (1), organic base is: one or more in triethylamine, trimethylamine, Isosorbide-5-Nitrae-diazabicylo [2.2.2] octane, pyridine, 4-methyl pyridine, nicotinic acid, isonicotinic acid.
Described organic base promotes REACTIVE DYES to react with the fixation on cellulose.
Described step (1), (2) Semi-polarity organic solvent are one or more in carbonic acid ester, dialkyl amide, little molecule oligomerization ether, sulfoxide type solvent.
Described carbonic acid ester is one or more in dimethyl carbonate, propene carbonate; Dialkyl amide is one or both of dimethylacetylamide, dimethyl formamide; Little molecule oligomerization ether is one or both in diethylene glycol dimethyl ether, triglyme; Sulfoxide type solvent is dimethyl sulfoxide (DMSO).
In described step (2), clean and carry out in dye bath or polar organic solvent, temperature is 80-130 ℃, and bath raio is 1:15-1:30, and each time is 10-40 minute, and wash number is 2-5 time.
Drying condition is vacuum 10-150mbar in described step (2), temperature 80-150 ℃, drying time 20-90min.
In described step (2), dyeing residual liquid is adjusted raffinate concentration to initial dye strength through adding solvent and supplementary dyestuff, and the alkali of supplementary respective amount makes pH identical with the dye bath of first preparation with electrical conductivity with electrolyte.
The invention discloses a kind of method of dying textile textiles in polar organic solvent with REACTIVE DYES.Use, without the organic solvent of nucleophilic activity, can thoroughly be avoided REACTIVE DYES and solvent reaction to cause invalid degraded, thereby realize the repeatedly circulating and recovering of dyeing residual liquid, makes zero-emission dyeing become possibility.Compare with water dyeing, the advantage of this method is to have avoided the invalid hydrolysis of dyestuff, and the very big degree of energy reduces the consumption of salt in dyeing.
Dye liquor after fixation of the present invention completes directly supplements appropriate dyestuff and alkaline agent can be reused for dyeing, the Δ E<1 of fabric changes of shade after dying in 10 circulations.Textiles can obtain DYED FABRICS finished product after organic solvent cleans, is dried.Do not use under the condition of color-fixing agent DYED FABRICS soaping fastness 4-5 level, dry friction COLOR FASTNESS 4-5 level, wet friction COLOR FASTNESS 3-5 level.
The present invention is by selecting suitable organic solvent to carry out High Temperature Pre swelling treatment to COTTON FABRIC, and by controlling kind, the consumption of electrolytical kind, consumption and organic base, promote Dye Adsorption and fixation, really realize REACTIVE DYES non-aqueous dyeing, from stopped the hydrolysis of dyestuff at all.Owing to not containing hydrolised dye in raffinate, its chemical constituent is basic not variation before and after dyeing, is only that concentration of component changes.The dyestuff consuming by complementary stain and auxiliary agent, can be directly again for dyeing.This technology can realize the repeatedly reuse of dye bath, final realization " zero-emission " is dyeed significant, meets the requirement of ecological spinning.
beneficial effect
(1) the present invention realizes real non-water dyeing, avoids the REACTIVE DYES cannot fixation because of hydrolysis in dyeing course, and the theoretical utilization rate of dyestuff can reach 100%;
(2) dyeing residual liquid of the present invention, not containing hydrolised dye, only needs directly to supplement dyestuff and auxiliary agent, can realize the reuse repeatedly of dye liquor.
The specific embodiment
Below in conjunction with specific embodiment, further set forth the present invention.Should be understood that these embodiment are only not used in and limit the scope of the invention for the present invention is described.In addition should be understood that those skilled in the art can make various changes or modifications the present invention after having read the content of the present invention's instruction, these equivalent form of values fall within the application's appended claims limited range equally.
Embodiment 1
Textile plain cloth 6.7g(is moved back to boil and float 40 * 40,133 * 72,123g/m
2) be immersed in 300mL dimethylacetylamide with 150 ℃ of pre-swellings 1 hour.By 0.3g CI Reactive Red 24,1.0g potassium nitrate and 1.0g pyridine are dissolved in 100mL dimethylacetylamide, and ultrasonic or heating obtains homogeneous dye liquor.The fabric that above-mentioned pre-swelling treatment is crossed is contaminated dye liquor, heats up and remains on 95 ℃ of dyeing 4 hours.After dye bath is cooling, after taking-up fabric is centrifugal, with 100mL dimethylacetylamide, clean and collect washing lotion, with 130 ℃, to clean 20 minutes, repeated washing process 3 times is until the clarification of dimethylacetylamide washing lotion is reclaimed dyestuff and auxiliary agent after merging washing lotion evaporation and concentration.Fabric after cleaning is through centrifugal, and at 130 ℃, 20mbar obtains DYED FABRICS to constant weight in dry 0.5 hour.DYED FABRICS K/S is 14,4 grades of fastnesss to washing, resistance to dry friction fastness 3-4 level, wet rubbing fastness 3-4 level.
Embodiment 2
Textile plain cloth 6.7g(is moved back to boil and float 40 * 40,133 * 72,123g/m2) be immersed in 300mL dimethylacetylamide with 120 ℃ of pre-swellings 4 hours.CI reactive black 5 by 0.6g after sulfuric ester is eliminated, 1.0g potassium nitrate and 2.0g pyridine are dissolved in 100mL dimethylacetylamide, and ultrasonic or heating obtains homogeneous dye liquor.The fabric that above-mentioned pre-swelling treatment is crossed is contaminated dye liquor, heats up and remains on 95 ℃ of dyeing 4 hours.After dye bath is cooling, after taking-up fabric is centrifugal, with 100mL dimethylacetylamide, clean and collect washing lotion, with 130 ℃, to clean 20 minutes, repeated washing process 2 times is until the clarification of dimethylacetylamide washing lotion is reclaimed dyestuff and auxiliary agent after merging washing lotion evaporation and concentration.Fabric after cleaning is through centrifugal, and at 130 ℃, 20mbar obtains DYED FABRICS to constant weight in dry 0.5 hour.DYED FABRICS K/S is 18,4 grades of fastnesss to washing, 5 grades of resistance to dry friction fastness, wet rubbing fastness 4-5 level.
Embodiment 3
Textile plain cloth 6.7g(is moved back to boil and float 40 * 40,133 * 72,123g/m2) be immersed in 300mL dimethylacetylamide with 80 ℃ of pre-swellings 24 hours.By 0.3g CI active red 120,0.5g potassium nitrate and 1.0g pyridine are dissolved in 100mL dimethylacetylamide, and ultrasonic or heating obtains homogeneous dye liquor.The fabric that above-mentioned pre-swelling treatment is crossed is contaminated dye liquor, heats up and remains on 95 ℃ of dyeing 4 hours.After dye bath is cooling, take out fabric and with 100mL dimethylacetylamide, cleans and collect washing lotion after centrifugal, with 130 ℃, to clean 20 minutes, repeated washing process 3 times or to the clarification of dimethylacetylamide washing lotion, reclaims dyestuff and auxiliary agent after merging washing lotion evaporation and concentration.In dyeing residual liquid, supplement dyestuff, salt, alkali to dyestuff initial concentration, repeat above-mentioned steps and carry out dyeing cycle 10 times.Fabric after above-mentioned cleaning, through centrifugal, at 130 ℃, 20mbar obtains DYED FABRICS to constant weight in dry 0.5 hour.The average K/S of DYED FABRICS is 16,4 grades of fastnesss to washing, 4 grades of resistance to dry friction fastness, wet rubbing fastness 3-4 level.The poor Δ E<1 of fabric coloured light after 10 dyeing.
Embodiment 4
Textile plain cloth 6.7g(is moved back to boil and float 40 * 40,133 * 72,123g/m2) be immersed in 300mL methyl-sulfoxide with 100 ℃ of pre-swellings 6 hours.By 0.3g CI reactive orange 5,1g potassium nitrate and 1.0g pyridine are dissolved in 100mL methyl-sulfoxide, and ultrasonic or heating obtains homogeneous dye liquor.The fabric that above-mentioned pre-swelling treatment is crossed is contaminated dye liquor, heats up and remains on 95 ℃ of dyeing 4 hours.After dye bath is cooling, take out fabric and with 100mL methyl-sulfoxide, cleans and collect washing lotion after centrifugal, to clean 30 minutes with 120 ℃, repeated washing process 3 times or to the clarification of methyl-sulfoxide washing lotion, reclaims dyestuff and auxiliary agent after merging washing lotion evaporation and concentration.In dyeing residual liquid, supplement dyestuff, salt, alkali to dyestuff initial concentration, repeat above-mentioned steps and carry out dyeing cycle 10 times.Fabric after above-mentioned cleaning, through centrifugal, at 140 ℃, 20mbar obtains DYED FABRICS to constant weight in dry 1 hour.The average K/S of DYED FABRICS is 14,4 grades of fastnesss to washing, resistance to dry friction fastness 3-4 level, wet rubbing fastness 3-4 level.Through 10 DYED FABRICS aberration Δ E<1.
Claims (8)
1. the anhydrous colouring method capable of circulation of REACTIVE DYES, comprising:
(1) dyestuff is added in polar organic solvent, then add electrolyte, organic base, dissolving, obtain dye bath; Wherein the proportionate relationship of dyestuff, polar organic solvent, electrolyte, organic base is 0.5-30g:1L:0-10g:0.1-30g;
(2) by pure cotton fabric in polar organic solvent, under 50 ℃ of-150 ℃ of conditions, pre-swelling 0.5-24h, then in above-mentioned dye bath, dye, dye bath ratio is 1:10-1:50, and dyeing temperature is 45-130 ℃, dyeing time is 0.5-3h, clean, be dried, obtain DYED FABRICS, wherein the proportionate relationship 6-7g:300ml of pure cotton fabric and polar organic solvent.
2. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, is characterized in that: in described step (1), dyestuff is s-triazine, vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class or halogen pyrimidines REACTIVE DYES.
3. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, is characterized in that: in described step (1), dyestuff is a kind of in CI active red, CI reactive black, CI active red, CI reactive orange.
4. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, is characterized in that: in described step (1), electrolyte is one or more in KI, sodium iodide, potassium bromide, sodium bromide, potassium nitrate, sodium nitrate, potassium dihydrogen phosphate, sodium dihydrogen phosphate, p-methyl benzenesulfonic acid sodium, p-methyl benzenesulfonic acid potassium, sodium tetrafluoroborate, sodium hexafluoro phosphate.
5. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, it is characterized in that: in described step (1), organic base is: one or more in triethylamine, trimethylamine, Isosorbide-5-Nitrae-diazabicylo [2.2.2] octane, pyridine, 4-methyl pyridine, nicotinic acid, isonicotinic acid.
6. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, is characterized in that: the polar organic solvent in described step (1), (2) is one or more in carbonic acid ester, dialkyl amide, little molecule oligomerization ether, sulfoxide type solvent.
7. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 6, is characterized in that: described carbonic acid ester is one or more in dimethyl carbonate, propene carbonate; Dialkyl amide is one or both of dimethylacetylamide, dimethyl formamide; Little molecule oligomerization ether is one or both in diethylene glycol dimethyl ether, triglyme; Sulfoxide type solvent is dimethyl sulfoxide (DMSO).
8. the anhydrous colouring method capable of circulation of a kind of REACTIVE DYES according to claim 1, it is characterized in that: in described step (2), clean and carry out in dye bath or polar organic solvent, temperature is 80-130 ℃; bath raio is 1:15~1:30; each time is 10-40 minute, and wash number is 2-5 time; Drying condition is vacuum 10-150mbar, temperature 80-150 ℃, drying time 20-90min.
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