CN103590267B - A kind of salt-free non-alkali dyeing method of non-water of vinylsulfone reactive dyes - Google Patents
A kind of salt-free non-alkali dyeing method of non-water of vinylsulfone reactive dyes Download PDFInfo
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Abstract
The present invention relates to a kind of salt-free non-alkali dyeing method of non-water of vinylsulfone reactive dyes, comprising: dyestuff is added in polar organic solvent, dissolve, obtain dye bath; Wherein the proportionate relationship of dyestuff and polar organic solvent is 0.5-30g:1L; Immersed by pure cotton fabric in polar organic solvent, under 35-180 DEG C of condition, pre-swelling treatment 0.5-24h, then immerse in dye bath and dye, temperature is 45-130 DEG C, and immerged time is 0.5-3h, and cleaning is dry, obtains DYED FABRICS.In the present invention, the dye bath of salt-free alkali-free enormously simplify the recycling of non-fixing dyes and the circulating and recovering of dye bath.
Description
Technical field
The invention belongs to colouring method field, particularly a kind of salt-free non-alkali dyeing method of non-water of vinylsulfone reactive dyes.Background technology
REACTIVE DYES emerged so far from 1956, is developed fast, be widely used in cellulose dyeing because chromatogram is complete, bright-colored, easy to use.On the other hand, along with the sternness increasingly of ecological environment problem, the problem that REACTIVE DYES causes is further outstanding.Containing the hydrolised dye of 30-40% in dyeing residual liquid, and the interpolation of a large amount of inorganic salts in dyeing course, both increase waste water treatment difficulty.
Dye in non-aqueous system, be considered to the environmental protection staining technique that greatly may reduce the non-water discharge of printing and dyeing.This type of studies multiplex critical carbon dioxide or rudimentary property halogenated hydrocarbon solvent as dyeing medium.Due to these media and the larger cellulose fibre of polarity and REACTIVE DYES compatibility poor, often poor effect in cellulose dyeing, need in system, introduce a small amount of water and dissolving (CHAVAN that is swelling and promotion dye material is carried out to cellulose fibre, R.B.andA.SUBRAMANIAN, dyeingcottonwithareactivedyefrompolar-nonpolarsolventsys tems.TextileResearchJournal, 1983.53:p.539; Sawada, K.andM.Ueda, Adsorptionandfixationofareactivedyeoncottoninnon ?aqueoussystems.Colorationtechnology, 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 a kind of salt-free non-alkali dyeing method of non-water of vinylsulfone reactive dyes, and this invention is salt-free non-alkali dyeing; This invention avoids the invalid hydrolysis of REACTIVE DYES in dyeing course, and reuse is simple, is conducive to dyeing and printing process and reduces discharging, even realize " zero-emission.
The salt-free non-alkali dyeing method of non-water of a kind of vinylsulfone reactive dyes of the present invention, comprising:
(1) vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES is added in polar organic solvent, dissolve, obtain dye bath; Wherein the proportionate relationship of dyestuff and polar organic solvent is 0.5-30g:1L;
(2) immerse in polar organic solvent by pure cotton fabric, under 35-180 DEG C of condition, pre-swelling treatment 0.5-24h, then immerse in dye bath and dye, temperature is 45-130 DEG C, and immerged time is 0.5-3h, and cleaning is dry, obtains DYED FABRICS.
Polar organic solvent in described step (1) is mixing polar organic solvent system.
Vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES in described step (1) is the single reaction group vinyl sulfone dyestuff through the process of desulfurization acid esters, two reactive group vinyl sulfone dyestuff, containing one or more in the hybrid reaction group active dye of vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) structure.
Described vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES is through desulfurization acid esters treatment step: CI reactive ethylene sulfone dyestuff and water ratio are 2-5g:50mL, by sodium bicarbonate and sodium carbonate buffer system, pH are adjusted to 7.5-9, at 30 DEG C-60 DEG C reaction 10-90 minute.After reaction terminates, pH is adjusted to neutrality, and obtains the vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES of cancellation sulfuric ester by the dimethylacetylamide DMAC that saltouts, dewaters, is dissolved in, filtration desalination and solvent evaporation.
Described step (2) Semi-polarity organic solvent is single polar solvent.
Described polar organic solvent is one or more in carbonic acid ester, dialkyl amide, Small molecular oligomerization ether, sulfoxide type solvents.Described carbonic acid ester is one or both in dimethyl carbonate, propene carbonate; Dialkyl amide is one or both in dimethylacetylamide, dimethyl formamide; Small molecular oligomerization ether is one or more in diethylene glycol dimethyl ether, triglyme; Sulfoxide type solvents is dimethyl sulfoxide (DMSO).
In described step (2), pre-swelling bath raio is 1:8-1:50, and temperature is 50-150 DEG C; Dye bath ratio is 1:8-1:50; Dyeing temperature is 50-100 DEG C.
In described step (2), cleaning for carry out in polar organic solvent, and cleaning temperature is 80-130 DEG C, and bath raio is 1:15-1:30, and scavenging period is 10-40 minute, and wash number is 2-5 time; Drying process condition is vacuum 10-150mbar, temperature 80-150 DEG C, drying time 20-90min.
Dyeing residual liquid in described step (2) after dyeing can directly again for dyeing to initial dye concentration through supplementing dyestuff.
In the present invention, the High Temperature Pre of textile textiles first in organic solvent through certain hour is swelling, then contaminate with the bath raio of 1:8-1:50 in the mixed organic solvents dye bath containing REACTIVE DYES, under 50-100 DEG C of condition, vinyl-sulfone reactive dyes and cotton fiber react fixation.Dye liquor after fixation completes can reuse after directly supplementing a certain amount of dyestuff.Textiles can obtain DYED FABRICS finished product after organic solvent cleaning, drying.Under not using 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 carries out High Temperature Pre swelling treatment by selecting suitable organic solvent to COTTON FABRIC, by to doing the process of desulfurization acid esters to commercialization vinyl sulfone dyestuff in advance, remove the necessity adding alkali in dye bath from, the chemical potential of dyestuff in dye bath is regulated by being mixed into poor solvent, remove necessity that salt adding is urged to contaminate from, really achieve the salt-free non-alkali dyeing of vinyl-sulfone reactive dyes, fundamentally stop the hydrolysis of dyestuff simultaneously.Owing to not containing hydrolised dye, salt or alkali in raffinate, the direct reuse of dyeing residual liquid can be realized by adding used up dyestuff.This technology fundamentally can avoid the discharge of reactive dyeing height salt, high-colour intensity wastewater, and dye bath reuse is simple to operation, dyes significant, meet the requirement of ecological spinning to final realization " zero-emission ".
beneficial effect
(1) the present invention is salt-free non-alkali dyeing;
(2) present invention, avoiding the invalid hydrolysis of REACTIVE DYES in dyeing course;
(3) reuse of the present invention is simple, is conducive to dyeing and printing process and reduces discharging, even realize " zero-emission ".
Detailed description of the invention
Below in conjunction with specific embodiment, set forth the present invention further.Should be understood that these embodiments are only not used in for illustration of the present invention to limit the scope of the invention.In addition should be understood that those skilled in the art can make various changes or modifications the present invention, and these equivalent form of values fall within the application's appended claims limited range equally after the content of having read the present invention's instruction.
Embodiment 1
5gCI reactive black 5 is dissolved in 50mL deionized water, adds sodium bicarbonate 3g, sodium carbonate 1g is adjusted to pH8.3, reacts 1 hour at 50 DEG C.Adding hydrogen chloride after reaction terminates regulates pH to neutral, adds anhydrous sodium sulfate and to saltout dyestuff, drying, be dissolved in by dried dyestuff filter-cakes in DMAC solution subsequently, filter, dried filtrate, obtains the CI reactive black 5 removing sulfuric ester.
Textile plain cloth 6.7g(is moved back and boils drift 40 × 40,133 × 72,123g/m
2) be immersed in 300mL dimethylacetylamide pre-swelling 1 hour with 150 DEG C.0.3g desulfurization acid esters CI reactive black 5 is dissolved in the mixed solution that 80mL diethylene glycol dimethyl ether and 20mL dimethylacetylamide form, ultrasonic or heating obtains homogeneous dye liquor.The fabric above-mentioned pre-swelling treatment crossed contaminates dye liquor, heats up and remains on 95 DEG C of dyeing 4 hours.Treat that dye bath cools, take out fabric centrifugal after clean with 100mL dimethylacetylamide and collects washing lotion, cleaning is 130 DEG C, 20 minutes, repeated washing process 3 times or to the clarification of dimethylacetylamide washing lotion, merging washing lotion also reclaims dyestuff after evaporation and concentration.Fabric after cleaning is through centrifugal, and at 130 DEG C, 20mbar drying 0.5 is little of constant weight, obtains DYED FABRICS.In dyeing residual liquid, supplement dyestuff to dyestuff initial concentration, repeat above-mentioned steps and circulate 10 times, DYED FABRICS K/S average 18, fastness to washing 4 grades, resistance to dry friction fastness 5 grades, wet rubbing fastness 4-5 level.Fabric aberration Δ E<1 after 10 dyeing.
Embodiment 2
5gCI reactive black 5 is dissolved in 50mL deionized water, adds sodium bicarbonate 3g, sodium carbonate 1g is adjusted to pH8.3, reacts 1 hour at 50 DEG C.Adding hydrogen chloride after reaction terminates regulates pH to neutral, adds anhydrous sodium sulfate and to saltout dyestuff, drying, be dissolved in by dried dyestuff filter-cakes in DMAC solution subsequently, filter, dried filtrate, obtains the CI reactive black 5 removing sulfuric ester.
Textile plain cloth 6.7g(is moved back and boils drift 40 × 40,133 × 72,123g/m
2) be immersed in 300mL dimethylacetylamide pre-swelling 1 hour with 150 DEG C.Be dissolved in 100mL dimethyl carbonate by 0.3g desulfurization acid esters CI reactive black 5, ultrasonic or heating obtains homogeneous dye liquor.The fabric above-mentioned pre-swelling treatment crossed contaminates dye liquor, heats up and remains on 75 DEG C of dyeing 4 hours.Treat that dye bath cools, clean with 100mL dimethylacetylamide after taking-up fabric is centrifugal and collect washing lotion, cleaning is 120 DEG C, 25 minutes, and repeated washing process 3 times, until the clarification of dimethylacetylamide washing lotion, merges washing lotion and also reclaims dyestuff after evaporation and concentration.Fabric after cleaning is through centrifugal, and at 130 DEG C, 20mbar drying 0.5 is little of constant weight, obtains DYED FABRICS.Dyeing residual liquid is by revolving steaming and be separated into reactive dye and residual solvent can directly again for dyeing.DYED FABRICS K/S average 18, fastness to washing 4 grades, resistance to dry friction fastness 5 grades, wet rubbing fastness 4-5 level.
Embodiment 3
20gCI active blue 19 is dissolved in 200mL deionized water, adds sodium bicarbonate 12g, sodium carbonate 4g is adjusted to pH8.3, reacts 1.5 hours at 50 DEG C.Adding hydrogen chloride after reaction terminates regulates pH to neutral, adds anhydrous sodium sulfate and to saltout dyestuff, drying, subsequently dried dyestuff filter-cakes to be dissolved in DMAC solution and filter, dried filtrate, obtain the CI active blue 19 removing sulfuric ester.
Textile plain cloth 6.7g(is moved back and boils drift 40 × 40,133 × 72,123g/m
2) be immersed in 300mL dimethyl sulfoxide (DMSO) pre-swelling 1 hour with 150 DEG C.Be dissolved in the mixed solvent of 90mL dimethyl carbonate and 10mL triglyme by 0.3g desulfurization acid esters CI active blue 19, ultrasonic or heating obtains homogeneous dye liquor.The fabric above-mentioned pre-swelling treatment crossed contaminates dye liquor, heats up and remains on 95 DEG C of dyeing 4 hours.Treat that dye bath cools, clean with 100mL dimethyl sulfoxide (DMSO) after taking-up fabric is centrifugal and collect washing lotion, cleaning is 120 DEG C, 25 minutes, and repeated washing process 3 times, until the clarification of dimethyl sulfoxide (DMSO) washing lotion, merges washing lotion and also reclaims dyestuff after evaporation and concentration.Fabric after cleaning is through centrifugal, and at 140 DEG C, dry 1 hour of 20mbar or to constant weight, obtains DYED FABRICS.In dyeing residual liquid, supplement dyestuff to dyestuff initial concentration, repeat above-mentioned steps and circulate 10 times, DYED FABRICS K/S average 17, fastness to washing 4 grades, resistance to dry friction fastness 5 grades, wet rubbing fastness 4 grades.Fabric aberration Δ E<1 after 10 dyeing.
Embodiment 4
20gCI active blue 19 is dissolved in 200mL deionized water, adds sodium bicarbonate 12g, sodium carbonate 4g is adjusted to pH8.3, reacts 1.5 hours at 50 DEG C.Adding hydrogen chloride after reaction terminates regulates pH to neutral, adds anhydrous sodium sulfate and to saltout dyestuff, drying, subsequently dried dyestuff filter-cakes to be dissolved in DMAC solution and filter, dried filtrate, obtain the CI active blue 19 removing sulfuric ester.
Textile plain cloth 6.7g(is moved back and boils drift 40 × 40,133 × 72,123g/m
2) be immersed in 300mL dimethyl sulfoxide (DMSO) pre-swelling 2 hours with 130 DEG C.Be dissolved in by 0.3g desulfurization acid esters CI active blue 19 in the mixed solvent of 50mL triglyme and 50mL propene carbonate composition, ultrasonic or heating obtains homogeneous dye liquor.The fabric above-mentioned pre-swelling treatment crossed contaminates dye liquor, heats up and remains on 115 DEG C of dyeing 3 hours.Treat that dye bath cools, clean with 100mL dimethyl sulfoxide (DMSO) after taking-up fabric is centrifugal and collect washing lotion, cleaning is 120 DEG C, 25 minutes, and repeated washing process 3 times, until the clarification of dimethyl sulfoxide (DMSO) washing lotion, merges washing lotion and also reclaims dyestuff after evaporation and concentration.Fabric after cleaning is through centrifugal, and at 140 DEG C, dry 1 hour of 20mbar or to constant weight, obtains DYED FABRICS.Dyeing residual liquid is by revolving steaming and be separated into reactive dye and residual solvent can directly again for dyeing.DYED FABRICS K/S average 18, fastness to washing 4 grades, resistance to dry friction fastness 5 grades, wet rubbing fastness 4 grades.
Claims (5)
1. the salt-free non-alkali dyeing method of the non-water of vinylsulfone reactive dyes, comprising:
(1) vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES is added in polar organic solvent, dissolve, obtain dye bath; Wherein the proportionate relationship of dyestuff and polar organic solvent is 0.5-30g:1L; Wherein vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) class REACTIVE DYES be through the single reaction group vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) of desulfurization acid esters process, two reactive group vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan), containing one or more in the hybrid reaction group active dye of vinyl sulfone(RemzaolHuo Xingranliaohuoxingjituan) structure;
(2) pure cotton fabric is immersed in polar organic solvent, under 35-180 DEG C of condition, pre-swelling treatment 0.5-24h, then immerse in dye bath and dye, temperature is 45-130 DEG C, and immerged time is 0.5-3h, and cleaning is dry, obtains DYED FABRICS; Wherein step (1), (2) Semi-polarity organic solvent are one or more in carbonic acid ester, dialkyl amide, Small molecular oligomerization ether, sulfoxide type solvents.
2. the salt-free non-alkali dyeing method of the non-water of a kind of vinyl sulfone dyestuff according to claim 1, is characterized in that: described carbonic acid ester is one or both in dimethyl carbonate, propene carbonate; Dialkyl amide is one or both in dimethylacetylamide, dimethyl formamide; Small molecular oligomerization ether is one or more in diethylene glycol dimethyl ether, triglyme; Sulfoxide type solvents is dimethyl sulfoxide (DMSO).
3. the salt-free non-alkali dyeing method of the non-water of a kind of vinyl sulfone dyestuff according to claim 1, it is characterized in that: in described step (2), pre-swelling bath raio is 1:8-1:50, temperature is 50-150 DEG C; Dye bath ratio is 1:8-1:50; Dyeing temperature is 50-100 DEG C.
4. the salt-free non-alkali dyeing method of the non-water of a kind of vinyl sulfone dyestuff according to claim 1, it is characterized in that: in described step (2), cleaning for carry out in polar organic solvent, cleaning temperature is 80-130 DEG C; bath raio is 1:15-1:30; scavenging period is 10-40 minute, and wash number is 2-5 time; Drying process condition is vacuum 10-150mbar, temperature 80-150 DEG C, drying time 20-90min.
5. the salt-free non-alkali dyeing method of the non-water of a kind of vinyl sulfone dyestuff according to claim 1, is characterized in that: the dyeing residual liquid in described step (2) after dyeing can directly again for dyeing to initial dye concentration through supplementing dyestuff.
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