CN109403099B - The synchronous non-aqueous dyeing method carried out of fixation is contaminated on high pitch black degree cotton fabric - Google Patents
The synchronous non-aqueous dyeing method carried out of fixation is contaminated on high pitch black degree cotton fabric Download PDFInfo
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- CN109403099B CN109403099B CN201811373624.2A CN201811373624A CN109403099B CN 109403099 B CN109403099 B CN 109403099B CN 201811373624 A CN201811373624 A CN 201811373624A CN 109403099 B CN109403099 B CN 109403099B
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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
- 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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- 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
- D06P1/64—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 low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/642—Compounds containing nitrogen
- D06P1/645—Aliphatic, araliphatic or cycloaliphatic compounds containing amino groups
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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
- D06P1/44—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
- D06P1/64—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 low-molecular-weight organic compounds without sulfate or sulfonate groups
- D06P1/642—Compounds containing nitrogen
- D06P1/649—Compounds containing carbonamide, thiocarbonamide or guanyl groups
- D06P1/6494—Compounds containing a guanyl group R-C-N=, e.g. (bi)guanadine, dicyandiamid amidines
-
- 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
- D06P1/90—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 organic solvents or aqueous emulsions thereof
- D06P1/92—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 organic solvents or aqueous emulsions thereof in organic solvents
- D06P1/928—Solvents other than hydrocarbons
Abstract
The invention discloses the synchronous non-aqueous dyeing method carried out of fixation is contaminated on a kind of high pitch black degree cotton fabric, this method includes being placed in cotton fabric in anhydrous dye bath to dye；Anhydrous dye bath is dissolved in anhydrous solvent by reactive dye to be obtained；Anhydrous solvent is made of ethylene glycol monomethyl ether acetate and aprotic polar solvent.This method includes that organic base is further added in anhydrous dye bath before heating starts.The non-aqueous dyeing method is able to solve discharge of wastewater caused by water-bath dyeing, improves the problems such as pitch black degree of black cotton fabric, and can provide the degree of fixation higher than the prior art, while can improve the dyefastness of non-aqueous dyeing.
Description
Technical field
The invention belongs to printing technology fields, are related to a kind of non-aqueous dyeing method of cotton fabric, more particularly, to a kind of high
The synchronous non-aqueous dyeing method carried out of fixation is contaminated on pitch black degree cotton fabric.
Background technique
Currently, cotton fabric dyeing process, which mainly passes through the hydroxyl on the reactive group and fabric fibre of reactive dye, carries out nucleophilic
Replace or addition reaction forms chemical bond.This is usually carried out in a water bath.Since hydrone also belongs to excellent nucleopilic reagent,
Cause in solution while there is also dyestuff hydrolysis or the competitive reactions of chemical bond rupture.In addition, usually requiring to carry out after dyeing
Fixation, common color fixing agent such as sodium carbonate, sodium phosphate are alkaline matter.This can be further exacerbated by the degree of dyestuff hydrolysis, lead
It causes dye fixing rate not high, the dyestuff of a large amount of non-fixation is remained in water-bath.It is such when cotton fabric contaminates shade especially black
For the degree of fixation of dyestuff usually only 60% or so, the dye quantity of waste is up to one third or more.
In addition, the problem of water-bath dyeing maximum causes Ecological Environment Risk to get worse in waste water.In dye bath, in addition to depositing
It further include promoting dye electrolyte and fixation alkali and other common dye materials, so as to cause chroma in waste water except a large amount of dyestuffs
High, salinity height, COD are high, and wastewater treatment difficulty is higher.Furthermore the cleaning step after fixation step needs to consume big
Clear water is measured, according to statistics, every 1kg cotton fabric averagely needs to consume the clear water of 50-110kg.It is useless that these clear water are equally converted into printing and dyeing
Water.
In order to solve the problems, such as the discharge of wastewater of cotton fabric dyeing process from source, in recent years, sight is gradually transferred to nothing by people
On water colouring method.Common non-aqueous dyeing method includes supercritical fluid dyeing, reverse micelle dyeing, vacuum sublimation dyeing, hangs
The dyeing of floating body system, organic solvent dyeing, etc..Having in common that for the above method is substituted using other solvents or fluid system
Water, or reduce the usage amount of water in dyeing course.Among these, more it is worth noting that supercritical fluid dyeing and organic solvent
Dyeing, these two types of colouring methods almost avoid the participation of water.
However, either supercritical fluid dyeing or organic solvent dye, few, dye that all there is suitable dyes types
Color system compatibility is bad, is difficult to the defects of contaminating shade.When cotton fabric contaminates shade especially black, this defect is especially
Obviously, the result is that apparent colour depth (i.e. pitch black degree) is difficult to improve caused by.If this defect can not solve, just it has been difficult to
At marketing.Because contaminating black for cotton fabric close to half dyestuff currently on the market.Solve the problems, such as that this can be borrowed merely
The thinking that water-bath of reflecting is dyed is contaminated shade by the way of reactive dye compound or improves pitch black degree, however, due to anhydrous
Dicyandiamide solution is totally different from water, and the properties such as the dissolubility and compatibility of dyestuff in different systems difference is larger, is difficult water
Bath dyes former class's transplanting and comes.In addition, organic solvent dyeing also needs to solve the problems, such as fixation and dyefastness.According to document
Investigate situation, not yet discovery in anhydrous solvent system using reactive dye compound solve dye shade and be capable of providing compared with
The document report of good dyefastness.
Therefore, there is an urgent need to make sustained improvement for existing non-aqueous dyeing method.
Summary of the invention
In view of the above drawbacks of the prior art, it is an object of the invention to solve discharge of wastewater caused by water-bath dyeing, dye
Shade, the pitch black degree for improving black cotton fabric, the degree of fixation for coordinating reactive dye compound, and improve the dye of non-aqueous dyeing
Color fastness, at least one of the especially most common colour fastness to rubbing and washing color fastness or a variety of.
Further, it is an object of the invention to solve discharge of wastewater caused by water-bath dyeing simultaneously, dye shade, improve
The problems such as pitch black degree of black cotton fabric.
Further, it is an object of the invention to solve discharge of wastewater caused by water-bath dyeing simultaneously, dye shade, mention
The pitch black degree of high black cotton fabric can simultaneously provide the problems such as degree of fixation comparable with the prior art.
Still further, it is an object of the invention to solve discharge of wastewater caused by water-bath dyeing simultaneously, dye shade, mention
The pitch black degree of high black cotton fabric can simultaneously provide the problems such as degree of fixation higher than the prior art.
And then further, it is deep it is an object of the invention to solve discharge of wastewater caused by water-bath dyeing, dye simultaneously
Tone, the pitch black degree for improving black cotton fabric, the degree of fixation for coordinating reactive dye compound, and improve the dyeing of non-aqueous dyeing
The problems such as fastness.
To solve the above-mentioned problems, the invention adopts the following technical scheme: dye fixation is same on a kind of high pitch black degree cotton fabric
The non-aqueous dyeing method that step carries out heats up this method comprises: cotton fabric is placed in anhydrous dye bath according to given pace, reaches
It is kept the temperature after target temperature, dyes certain time；It is cooled to room temperature after dyeing, cleans dyed fabric using anhydrous solvent, most
After be dried to obtain dyed cotton fabric；Wherein, the anhydrous dye bath is dissolved in anhydrous solvent by reactive dye obtains, described anhydrous
Solvent is made of ethylene glycol monomethyl ether acetate and aprotic polar solvent；It is characterized in that, the method includes heatings to start
It is preceding that organic base is further added in the anhydrous dye bath.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the aprotic polar solvent is selected from dimethyl sulfoxide, diformazan
Base formamide, dimethyl acetamide, sulfolane, acetonitrile and acetone the mixture of any one or more.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the aprotic polar solvent is selected from dimethyl sulfoxide, diformazan
The mixture of any one or more of base formamide and dimethyl acetamide.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the aprotic polar solvent is selected from dimethyl sulfoxide.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the volume of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide
Than for (55-80): (45-20).
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the volume of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide
Than for (65-75): (35-25).
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the organic base is selected from triethylene diamine and tetramethylguanidine
Mixture.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the weight ratio of triethylene diamine and tetramethylguanidine is (1.5-
2): 1.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the additional amount of the organic base is 2-8g/L.
Non-aqueous dyeing method above-mentioned according to the present invention, wherein the cotton fabric first passes through dimethyl sulfoxide swelling in advance.
Reactive dye
As reactive dye of the invention, it is selected from active black dye composition.
Further, active black dye composition includes dye composition A, wherein dye composition A is selected from formula (I) institute
Any one or more of the dye composition shown；
In formula (I), R1-R4It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y1-Y2It is respectively independent
Ground is selected from SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K.
Further, further, active black dye composition further includes dye composition B and dye composition C；Its
In,
Dye composition B is selected from any one or more of dye composition shown in formula (II)；
In formula (II), R5-R8It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y3-Y4Respectively solely
On the spot it is selected from SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Dye composition C is selected from any one or more of dye composition shown in formula (III)；
In formula (III), R9-R10It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y5Independently select
From SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K.
In a preferred embodiment, dye composition A be selected from formula (I ') shown in dye composition any one or
It is a variety of；
In formula (I '), Y1-Y2It is each independently selected from SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Dye composition B is selected from any one or more of dye composition shown in formula (II ')；
In formula (II '), R6Selected from SO3M；R7-R8It is each independently selected from C1-C4Alkyl and C1-C4Alkoxy；Y3-Y4Respectively
From independently selected from SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Dye composition C is selected from any one or more of dye composition shown in formula (III ')；
In formula (III), Y5Independently selected from SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K.
In a specific embodiment, dye composition A is selected from dye composition shown in formula (I-1),
In another particular embodiment of the invention, dye composition A is selected from dye composition shown in formula (I-2),
In a specific embodiment, dye composition B is selected from dye composition shown in formula (II-1),
In another particular embodiment of the invention, dye composition B is selected from dye composition shown in formula (II-2),
In a specific embodiment, dye composition C is selected from dye composition shown in formula (III-1),
In another particular embodiment of the invention, dye composition C is selected from dye composition shown in formula (III-2),
In the present invention, dye composition is originated from known product in the market, can also be prepared according to known method.
Most preferably, dye composition A of the invention, dye composition B and dye composition C are selected from shown in formula (I-1)
Dye composition, dye composition shown in dye composition, formula (III-1) shown in formula (II-1).
Certainly, those skilled in the art know, dye composition shown in formula (I-2), formula (II- can be used
2) dye composition shown in dye composition, formula shown in (III-2) substitutes above-mentioned dye composition, because they are in alkalinity
Under the conditions of can be converted into dye composition shown in dye composition shown in formula (I-1), formula (II-1), formula (III-1) institute
The dye composition shown.
Advantageously, when using dye composition, formula (III- shown in dye composition, formula (II-2) shown in formula (I-2)
2) shown in when dye composition, vinyl sulfone dyestuff compound is being formed it into using preceding plus alkali, is then being analysed in neutral conditions
Out.After crude product is extracted using organic solvent, vacuum distillation obtains the vinyl sulfone dyestuff compound of high-purity.
It further, mainly include dye composition A, dye composition B as active black dye composition of the invention
With dye composition C.
It in the above-described embodiment, " mainly include " typicallying represent except dye composition A, dye composition B and dyestuff
It closes and also optionally includes other dye components other than object C；But dye composition A, dye composition B and dye composition C are accounted for
70% or more of the sum of all dye component weight, preferably 80% or more, more preferable 90% or more, and most preferably 95% with
On.
In a preferred embodiment, " mainly including " indicates dye composition A, dye composition B and dye composition C
Total weight and active black dye composition weight ratio be not less than 90%；Preferably not less than 95%；More desirably not less than
97%；And most desirably not less than 98%.
In further preferred embodiment, as active black dye composition of the invention, by dye composition A,
Dye composition B and dye composition C composition.That is, as active black dye composition of the invention, by dyestuff chemical combination
Object A, dye composition B and dye composition C are mixed.
Advantageously, mixing can take dry mixed, can also take wet-mixing.
In the embodiment of dry mixed, each dye composition is taken to be made by extrusion molding comminution granulation or spray drying
The dye granule that grain method obtains carries out dry type mixing.Advantageously, the partial size of dye granule is 100-2000 μm, preferably 150-1500
μm, more preferable 200-1000 μm, and, most preferably 200-500 μm.
In the embodiment of wet-mixing, slurries are proportionally made in each dye composition, cooking-pot type stirring stirring is spelled
After marriage, it is spray-dried.
Total weight based on active black dye composition calculates, and the weight percent of dye composition A is 45-85%.
The total weight for being preferably based on active black dye composition calculates, and the weight percent of dye composition A is 50-
80%.
It is highly preferred that the total weight based on active black dye composition calculates, the weight percent of dye composition A is
55-75%.
And most preferably, the total weight based on active black dye composition calculates, the weight percent of dye composition A
Than for 60-70%.
In a specific embodiment, the total weight based on active black dye composition calculates, dye composition A's
Weight percent is 65%.
Total weight based on active black dye composition calculates, and the weight percent of dye composition B is 15-35%.
The total weight for being preferably based on active black dye composition calculates, and the weight percent of dye composition B is 18-
32%.
It is highly preferred that the total weight based on active black dye composition calculates, the weight percent of dye composition B is
20-30%.
And most preferably, the total weight based on active black dye composition calculates, the weight percent of dye composition B
Than for 22-28%.
In a specific embodiment, the total weight based on active black dye composition calculates, dye composition B's
Weight percent is 25%.
Total weight based on active black dye composition calculates, and the weight percent of dye composition C is 5-18%.
The total weight for being preferably based on active black dye composition calculates, and the weight percent of dye composition C is 6-
16%.
It is highly preferred that the total weight based on active black dye composition calculates, the weight percent of dye composition C is 7-
14%.
And most preferably, the total weight based on active black dye composition calculates, the weight percent of dye composition C
Than for 8-12%.
In a specific embodiment, the total weight based on active black dye composition calculates, dye composition C's
Weight percent is 10%.
Anhydrous solvent
As anhydrous solvent of the invention, mainly it is made of ethylene glycol monomethyl ether acetate and aprotic polar solvent.
In the present invention, " mainly by ... form " indicates that anhydrous solvent is removed including ethylene glycol monomethyl ether acetate and non-proton
Other organic solvents, but the body of ethylene glycol monomethyl ether acetate and aprotic polar solvent are also optionally included other than polar solvent
The sum of product accounts for 90% or more of the sum of all solvent volumes, preferably 95% or more, more preferable 97% or more, and most preferably
98% or more.In one embodiment, the volume of ethylene glycol monomethyl ether acetate is 65 unit volumes, aprotic polar solvent
Volume be 30 unit volumes, the volumes of other organic solvents is 5 unit volumes.
Advantageously, the volume ratio of ethylene glycol monomethyl ether acetate and aprotic polar solvent is (55-80): (45-20).It is excellent
The volume ratio of selection of land, ethylene glycol monomethyl ether acetate and aprotic polar solvent is (60-80): (40-20)；It is highly preferred that second
The volume ratio of glycol monomethylether acetate and aprotic polar solvent is (65-80): (35-20)；And most preferably, second two
The volume ratio of alcohol methyl ether acetate and aprotic polar solvent is (65-75): (35-25).
In a specific embodiment, the volume ratio of ethylene glycol monomethyl ether acetate and aprotic polar solvent is
70:30.
In a preferred embodiment, anhydrous solvent of the invention is molten by ethylene glycol monomethyl ether acetate and aprotonic polar
Agent composition.
As aprotic polar solvent of the invention, including dimethyl sulfoxide, dimethylformamide, dimethyl acetamide, ring
Fourth sulfone, acetonitrile, acetone and hexamethyl phosphoramide.
Preferably, the aprotic polar solvent is selected from dimethyl sulfoxide, dimethylformamide, dimethyl acetamide, ring fourth
The mixture of any one or more of sulfone, acetonitrile and acetone.
It is highly preferred that the aprotic polar solvent is selected from dimethyl sulfoxide, dimethylformamide, dimethyl acetamide, ring
The mixture of any one or more of fourth sulfone and acetonitrile.
And most preferably, the aprotic polar solvent is selected from dimethyl sulfoxide, dimethylformamide and dimethylacetamide
The mixture of any one or more of amine.
In a specific embodiment, the aprotic polar solvent is selected from dimethyl sulfoxide.
As other organic solvents of the invention, including but not limited to, aromatic hydrocarbon solvent, fat hydrocarbon solvent, alicyclic ring
Hydrocarbon solvent, halogenated hydrocarbon solvent, alcohols solvent, ether solvent, esters solvent, ketones solvent, polyalcohols solvent and remaining
Solvent.
It as aromatic hydrocarbon solvent, such as can enumerate, benzene, toluene, ethylbenzene, ortho-xylene, meta-xylene and paraxylene,
Etc..
It as fat hydrocarbon solvent, such as can enumerate, the petroleum ether of pentane, hexane, octane and boiling point at 60-90 DEG C, etc.
Deng.
It as alicyclic hydrocarbon type solvent, such as can enumerate, pentamethylene, hexamethylene, cyclohexanone, toluene cyclohexanone, etc..
It as halogenated hydrocarbon solvent, such as can enumerate, chlorobenzene, o-dichlorohenzene, m-dichlorobenzene, paracide, bromobenzene, dichloro
Methane, chloroform, etc..
It as alcohols solvent, such as can enumerate, methanol, ethyl alcohol, propyl alcohol, isopropanol, butanol, isobutanol, etc..
It as ether solvent, such as can enumerate, methyl ether, ether, ethyl methyl ether, propylene oxide, tetrahydrofuran, dioxane,
Etc..
It as esters solvent, such as can enumerate, methyl formate, Ethyl formate, methyl acetate, ethyl acetate, propyl acetate,
Etc..
It as ketones solvent, such as can enumerate, acetone, methyl ethyl ketone, methyl isopropyl ketone, methyl n-butyl ketone, methyl are different
Butanone, etc..
As polyalcohols solvent, such as can enumerate, ethylene glycol, glycerine, ethylene glycol, monomethyl ether, ethylene glycol monoethyl ether,
Ethylene glycol ether, ethylene glycol monobutyl ether, glycol dimethyl ether, ethylene glycol diethyl ether, ethylene glycol dipropyl ether, two fourth of ethylene glycol
Ether, etc..
It as remaining solvent, such as can enumerate, dimethyl carbonate, phenol, etc..
In view of anhydrous solvent system of the invention and the mechanism of dye fixing, as other organic solvents, principle with
Dye fixing reaction is not interfered to be preferred.This kind of solvent can be considered atent solvent.In a specific embodiment, the inertia
Solvent can be acetone.In another particular embodiment of the invention, the atent solvent can be dioxane.
However, anhydrous solvent of the invention is by ethylene glycol monomethyl ether acetate and two as highly preferred embodiment
First sulfoxide composition.That is, as anhydrous solvent of the invention, by ethylene glycol monomethyl ether acetate and dimethyl sulfoxide mixing
At.
It is not intended to limited to any theory, anhydrous solvent system of the invention eliminates the hydrolysis of disperse black dye composition
Reaction, improves the dye-uptake and degree of fixation of dyestuff to a certain extent.
Advantageously, the volume ratio of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide is (55-80): (45-20).Preferably,
The volume ratio of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide is (60-80): (40-20)；It is highly preferred that glycol monoethyl ether second
The volume ratio of acid esters and dimethyl sulfoxide is (65-80): (35-20)；And most preferably, ethylene glycol monomethyl ether acetate and two
The volume ratio of first sulfoxide is (65-75): (35-25).
In a specific embodiment, the volume ratio of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide is 70:30.
The anhydrous solvent system of above-mentioned specific composition further improves dye fixing rate of the invention.
Fixation alkali
In the methods of the invention, considered based on fixation and raising dyeability, be preferably added to fixation alkali.
It theoretically can be inorganic base as fixation alkali of the invention, be also possible to organic base.
As inorganic base, sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two can be
Sodium, dipotassium hydrogen phosphate, sodium pyrophosphate, potassium pyrophosphate, sodium hydroxide, potassium hydroxide, sodium tripolyphosphate, potassium tripolyphosphate, six are partially
Sodium phosphate and hexa metaphosphoric acid potassium and its mixture.
Preferably, inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two
Sodium, dipotassium hydrogen phosphate, sodium pyrophosphate, potassium pyrophosphate and its mixture.
It is highly preferred that inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two
Sodium, dipotassium hydrogen phosphate and its mixture.
And most preferably, inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate and its mixture.
Dye fixing rate, but inorganic base solubility in anhydrous solvent system of the invention can be improved in the addition of inorganic base
It is limited；In addition, inorganic base improves limitation to dye fixing rate of the invention under identical concentration levels.Therefore, as
Fixation alkali of the invention, preferably organic base；It or mainly include organic base.
In one embodiment, as fixation alkali of the invention, preferably organic base.
As organic base of the invention, it is selected from triethylene diamine, tetramethylguanidine, hexa and its mixture.
In the present invention, the addition of organic base can significantly improve dye fixing rate of the invention.Organic base is not being used
In the case where, used reactive dye and anhydrous solvent are depended only on, is knitted although the high cotton without blackness can also be obtained
Object, but dye fixing rate is lower, only 10% or so.This will lead to that dyeing efficiency is not high, and dye loss is serious.Have in use
In the case where machine alkali, if only then dye fixing rate highest can achieve 65% or so using triethylene diamine；If only
Using only tetramethylguanidine, then dye fixing rate highest can achieve 60% or so；And if only being contaminated using hexa
Color degree of fixation is typically in 30-40% or so.
It is therefore preferred that being selected from triethylene diamine, tetramethylguanidine and its mixture as organic base of the invention.
When using these organic bases, dye fixing rate of the invention and existing water phase dyeing are at least suitable, or obvious high
In the prior art.
In order to further increase dyeing efficiency, need to combine the optimization of anhydrous solvent system composition, by using triethylene
Diamines and the mixture of tetramethylguanidine are just able to achieve significantly improving for dye fixing rate as fixation alkali.Inventors have found that passing through
When the weight ratio of adjustment triethylene diamine and tetramethylguanidine is within the scope of special value, in the identical situation of other technological parameters
Under, dye fixing rate of the invention can be optimized between 70-80%.
Advantageously, in triethylene diamine and the mixture of tetramethylguanidine, the weight ratio of triethylene diamine and tetramethylguanidine
For (1.5-2): 1, preferably (1.5-1.9): 1, more preferably (1.5-1.8): 1, and, most preferably (1.5-1.7): 1.
In a specific embodiment, fixation alkali is selected from the mixture of triethylene diamine and tetramethylguanidine, wherein three
The weight ratio of ethylene diamine and tetramethylguanidine is 1.6:1.
It is not intended to limited to any theory, is carried out in anhydrous solvent due to dyeing, the organic base of specific composition of the present invention
Interaction is generated respectively with dye composition A of the invention, dye composition B and dye composition C, finally promotes dispersion
Hydroxyl on black dye composition and cotton fiber carries out nucleophilic addition or nucleophilic substitution.In contrast, triethylene diamine is more
The degree of fixation for being conducive to dye composition A improves；And tetramethylguanidine is more advantageous to consolidating for dye composition B and dye composition C
Color rate improves.
On the other hand, for the effect in terms of dyefastness, the organic base of specific composition of the present invention is for smooth cotton fabric
Fiber and enhancing dye-fibre interaction equally exist larger effect.Test result shows colour fastness to rubbing and water-fastness
Color fastness increases.
It in another embodiment, mainly include organic base as fixation alkali of the invention.
In the above-described embodiment, " mainly including " it is other organic to indicate that fixation alkali also optionally includes in addition to organic base
Alkali and inorganic base；But the weight of organic base accounts for 90% or more of the sum of all fixation alkali weight, and preferably 95% or more, more preferably
97% or more, and most preferably 98% or more.Preferably, fixation alkali also optionally includes mentioned-above nothing in addition to organic base
Machine alkali.
As inorganic base, sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two can be
Sodium, dipotassium hydrogen phosphate, sodium pyrophosphate, potassium pyrophosphate, sodium hydroxide, potassium hydroxide, sodium tripolyphosphate, potassium tripolyphosphate, six are partially
Sodium phosphate and hexa metaphosphoric acid potassium and its mixture.
Preferably, inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two
Sodium, dipotassium hydrogen phosphate, sodium pyrophosphate, potassium pyrophosphate and its mixture.
It is highly preferred that inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate, sodium metasilicate, potassium silicate, phosphoric acid hydrogen two
Sodium, dipotassium hydrogen phosphate and its mixture.
And most preferably, inorganic base is selected from sodium carbonate, sodium phosphate, potassium carbonate, potassium phosphate and its mixture.
In a specific embodiment, fixation alkali is selected from the mixture of triethylene diamine, tetramethylguanidine and sodium carbonate.
Advantageously, in the mixture of triethylene diamine, tetramethylguanidine and sodium carbonate, triethylene diamine, tetramethylguanidine and
The weight ratio of sodium carbonate is (1.5-2): 1:(0.01-0.3), preferably (1.5-1.9): 1:(0.01-0.25), more preferably
(1.5-1.8): 1:(0.01-0.2), and, most preferably (1.5-1.7): 1:(0.01-0.15).
In one more specifically embodiment, fixation alkali is selected from the mixed of triethylene diamine, tetramethylguanidine and sodium carbonate
Object is closed, the weight ratio of triethylene diamine, tetramethylguanidine and sodium carbonate is 1.5:1:0.1.
Colouring method
As colouring method of the invention, it is to be placed in cotton fabric in anhydrous dye bath, heats up according to given pace, reaches mesh
It is kept the temperature after mark temperature, dyes certain time；It is cooled to room temperature after dyeing, cleans dyed fabric using anhydrous solvent, finally
It is dried to obtain dyed cotton fabric.
Anhydrous dye bath is dissolved in anhydrous solvent above-mentioned by reactive dye above-mentioned (or active black dye composition)
It obtains.
In the present invention, the bath raio of the cotton fabric (dry weight) and anhydrous dye bath is 1:(8-25) g/mL.
Preferably, the cotton fabric and the bath raio of anhydrous dye bath are 1:(10-22) g/mL；It is highly preferred that the cotton fabric
Bath raio with anhydrous dye bath is 1:(12-20) g/mL；And most preferably, the cotton fabric and the bath raio of anhydrous dye bath are 1:
(14-18)g/mL。
In a specific embodiment, the cotton fabric and the bath raio of anhydrous dye bath are 1:16g/mL.
In the present invention, dye dosage 2-6o.w.f%.
Specifically, dye dosage 2o.w.f%, 3o.w.f%, 4o.w.f%, 5o.w.f%, 6o.w.f%.
Preferably, dye dosage 2-5o.w.f%；It is highly preferred that dye dosage is 3-5o.w.f%.
In a specific embodiment, dye dosage 4o.w.f%.
In the present invention, the heating rate of dyeing is 0.5-5 DEG C/min.
Preferably, the heating rate is 1-4.5 DEG C/min；It is highly preferred that the heating rate is 1.5-4 DEG C/min；
And most preferably, the heating rate is 2-3.5 DEG C/min.
In a specific embodiment, the heating rate is 3 DEG C/min.
In the present invention, the target temperature of dyeing is 70-100 DEG C.
Preferably, the target temperature is 75-95 DEG C；It is highly preferred that the target temperature is 80-95 DEG C；And it is optimal
Selection of land, the target temperature are 80-90 DEG C.
In a specific embodiment, the target temperature is 85 DEG C.
In the present invention, dyeing time 1-12h.
Preferably, the dyeing time is 2-10h；It is highly preferred that the dyeing time is 3-8h；And most preferably,
The dyeing time is 4-6h.
In a specific embodiment, the dyeing time is 5h.
It in the present invention, further comprise that the step of fixation alkali carries out fixation is added.
As fixation alkali of the invention, preferably organic base；It or mainly include organic base.
After dyeing terminates to be cooled to room temperature, advantageously, ethylene glycol monomethyl ether acetate and aprotonic polar are used respectively
Solvent respectively cleans more than once, preferably more than twice, until to the last a cleaning solution is colourless.
In a specific embodiment, after dyeing terminates to be cooled to room temperature, glycol monoethyl ether second is used respectively
Acid esters and dimethyl sulfoxide respectively clean more than once, preferably more than twice, until to the last a cleaning solution is colourless.
More advantageously, the dimethyl sulfoxide of ethylene glycol monomethyl ether acetate and heat that heat is used alternatingly respectively cleans more than once,
It is preferred that more than twice, until to the last a cleaning solution is colourless.
Hereinbefore, " hot " temperature indicated between 40-60 DEG C, the temperature preferably between 45-55 DEG C.
In a specific embodiment, " hot " to indicate 50 DEG C.
Advantageously as the cotton fabric that the above method uses, dimethyl sulfoxide swelling is first passed through in advance.Preferably, cotton fabric
Swellbility is between 10-30%, more preferably in 15-30%, and, most preferably between 20-30%.
In a specific embodiment, the swellbility of cotton fabric is 22%.
The dipping preferred 1-6h of 0.5-12h is obtained preferably at 60-90 DEG C preferably 70-90 DEG C for the swelling of cotton fabric.
In swelling, bath raio is advantageously 1:(10-50)；Preferably, bath raio is advantageously 1:(15-45)；It is highly preferred that
Bath raio is advantageously 1:(20-40)；And most preferably, bath raio is advantageously 1:(25-35).
In a specific embodiment, the swelling of cotton fabric impregnates 4h at 80 DEG C and obtains, bath raio 1:30.According to
It is 22% that centrifugation weight method, which measures its swellbility,.
In one preferred embodiment, when using fixation alkali and when fixation alkali is organic base above-mentioned, the present invention
The synchronous colouring method carried out of dye fixation on a kind of cotton fabric is additionally provided, in nothing above-mentioned before starting the method includes heating
Organic base above-mentioned is further added in water dye bath.
In the present invention, the additional amount of organic base is 2-8g/L.Preferably, the additional amount of organic base is 3-8g/L；It is more excellent
Selection of land, the additional amount of organic base are 4-8g/L；And most preferably, the additional amount of organic base is 5-8g/L.
In a specific embodiment, the additional amount of organic base is 6g/L.
Advantageously as the cotton fabric that the above method uses, dimethyl sulfoxide swelling is first passed through in advance.Preferably, cotton fabric
Swellbility is between 10-30%, more preferably in 15-30%, and, most preferably between 20-30%.
In a specific embodiment, the swellbility of cotton fabric is 22%.
The swelling of cotton fabric is carried out according to preceding method.
In another preferred embodiment, when using fixation alkali and when fixation alkali mainly includes organic base above-mentioned
When, the present invention also provides the colouring methods that fixation substep progress is contaminated on a kind of cotton fabric, and the method includes reaching target temperature
Fixation alkali above-mentioned is further added after degree in anhydrous dye bath above-mentioned.
In the present invention, the additional amount of fixation alkali is 2-8g/L.Preferably, the additional amount of fixation alkali is 3-8g/L；It is more excellent
Selection of land, the additional amount of fixation alkali are 4-8g/L；And most preferably, the additional amount of fixation alkali is 5-8g/L.
In a specific embodiment, the additional amount of fixation alkali is 6g/L.
Advantageously as the cotton fabric that the above method uses, dimethyl sulfoxide swelling is first passed through in advance.Preferably, cotton fabric
Swellbility is between 10-30%, more preferably in 15-30%, and, most preferably between 20-30%.
In a specific embodiment, the swellbility of cotton fabric is 22%.
The swelling of cotton fabric is carried out according to preceding method.
It is not intended to limited to any theory, the effect that swelling is conducive to improve between cotton-textile fibres and reactive dye is imitated
Fruit to improve dye fixing rate of the invention, while also contributing to further improving washing fastness.
Specific embodiment
The invention will be further elucidated with reference to specific embodiments.
It should be understood that a specific embodiment of the invention is only used for illustrating the spirit and principles in the present invention, rather than limitation
The scope of the present invention.In addition, it should also be understood that, after reading the contents of the present invention, those skilled in the art can be to of the invention
Technical solution make it is various change, replace, delete, correct or adjust, these equivalents thereofs equally fall within right of the present invention
Claim limited range.
In the present invention, the swellbility of cotton fabric is carried out by centrifugation weight method.Specific practice is: the cotton after swelling is knitted
Object is dry to constant weight after being centrifuged, and measures increase percentage % of its weight relative to cotton fabric dry weight before swell process, as
Swellbility.
The measurement of apparent colour depth Integ value carries out on Datacolor color measurement and color match instrument, and dyed fabric is built up 4
Layer, every layer of front and back sides take a point, measure 8 points and be averaged.
Degree of fixation include each dye component degree of fixation and two kinds of absolute degree of fixation.The former is by measuring each dye component most
Molar absorption coefficient at big absorbing wavelength and the absorbance before and after fixation simultaneously use maximum absorption wavelength-equation solving approach meter
The dye strength before and after each dye component fixation is calculated to be calculated.The degree of fixation and its weight ratio that the latter passes through each dye component
It is calculated after example weighting.In the present invention, when not indicating the situation of specific dye component, the degree of fixation is the latter.
Colour fastness to rubbing and washing color fastness (60 DEG C) respectively according to associated international standards ISO105-X12 and
ISO105-C10 measurement.
Embodiment 1
By dye composition, 10% formula shown in dye composition shown in 65% formula (I-1), 25% formula (II-1)
(III-1) dye composition shown in mixes active black dye composition.Active black dye composition is dissolved in volume
Dye bath is obtained in anhydrous solvent than ethylene glycol monomethyl ether acetate and dimethyl sulfoxide for 70:30.Then by triethylene diamine
Anhydrous dye bath is added with the mixture of tetramethylguanidine, the weight ratio of the two is 1.6:1；The additional amount of organic base is 6g/L.Ultrasound
Obtain uniform anhydrous dye bath.The cotton fabric for first passing through dimethyl sulfoxide swelling in advance and swellbility is 22% is put into anhydrous dye bath.
Cotton fabric and the bath raio of anhydrous dye bath are 1:16g/mL.Dye dosage is 4o.w.f%.It heats up, arrives according to the rate of 3 DEG C/min
It is kept the temperature after up to 85 DEG C of target temperature, dyes 5h；It is cooled to room temperature after dyeing, 50 DEG C of glycol monoethyl ether second is used alternatingly
Acid esters and 50 DEG C of dimethyl sulfoxide respectively clean 3 times, and each dosage is 20mL, are finally dried to obtain dyed cotton fabric.
Embodiment 2
By dye composition shown in dye composition shown in 70% formula (I-1), 22% formula (II-1), 8% formula (III-
1) dye composition shown in mixes active black dye composition.Active black dye composition, which is dissolved in volume ratio, is
Dye bath is obtained in the ethylene glycol monomethyl ether acetate of 65:35 and the anhydrous solvent of dimethyl sulfoxide.Then by triethylene diamine and four
Anhydrous dye bath is added in the mixture of methylguanidine, and the weight ratio of the two is 1.8:1；The additional amount of organic base is 8g/L.Ultrasound obtains
Uniform anhydrous dye bath.The cotton fabric for first passing through dimethyl sulfoxide swelling in advance and swellbility is 22% is put into anhydrous dye bath.Cotton is knitted
Object and the bath raio of anhydrous dye bath are 1:18g/mL.Dye dosage is 4o.w.f%.It heats up according to the rate of 3 DEG C/min, reaches mesh
It is kept the temperature after 90 DEG C of temperature of mark, dyes 4h；It is cooled to room temperature after dyeing, 50 DEG C of ethylene glycol monomethyl ether acetate is used alternatingly
Dimethyl sulfoxide with 50 DEG C respectively cleans 3 times, and each dosage is 20mL, is finally dried to obtain dyed cotton fabric.
Embodiment 3
By dye composition, 12% formula shown in dye composition shown in 60% formula (I-1), 28% formula (II-1)
(III-1) dye composition shown in mixes active black dye composition.Active black dye composition is dissolved in volume
Dye bath is obtained in anhydrous solvent than ethylene glycol monomethyl ether acetate and dimethyl sulfoxide for 75:25.Then by triethylene diamine
Anhydrous dye bath is added with the mixture of tetramethylguanidine, the weight ratio of the two is 1.5:1；The additional amount of organic base is 5g/L.Ultrasound
Obtain uniform anhydrous dye bath.The cotton fabric for first passing through dimethyl sulfoxide swelling in advance and swellbility is 22% is put into anhydrous dye bath.
Cotton fabric and the bath raio of anhydrous dye bath are 1:14g/mL.Dye dosage is 4o.w.f%.It heats up, arrives according to the rate of 3 DEG C/min
It is kept the temperature after up to 80 DEG C of target temperature, dyes 6h；It is cooled to room temperature after dyeing, 50 DEG C of glycol monoethyl ether second is used alternatingly
Acid esters and 50 DEG C of dimethyl sulfoxide respectively clean 3 times, and each dosage is 20mL, are finally dried to obtain dyed cotton fabric.
Embodiment 4
By dye composition, 10% formula shown in dye composition shown in 65% formula (I-1), 25% formula (II-1)
(III-1) dye composition shown in mixes active black dye composition.Active black dye composition is dissolved in volume
Dye bath is obtained in anhydrous solvent than ethylene glycol monomethyl ether acetate and dimethyl sulfoxide for 70:30.Ultrasound obtains uniform anhydrous
Dye bath.The cotton fabric for first passing through dimethyl sulfoxide swelling in advance and swellbility is 22% is put into anhydrous dye bath.Cotton fabric with it is anhydrous
The bath raio of dye bath is 1:16g/mL.Dye dosage is 4o.w.f%.It heats up according to the rate of 3 DEG C/min, reaches target temperature 85
It is kept the temperature after DEG C, anhydrous dye bath then is added in the mixture of triethylene diamine, tetramethylguanidine and sodium carbonate, the weight ratio of three is
1.5:1:0.1.The additional amount of fixation alkali is 6g/L.Dye 5h.It is cooled to room temperature after dyeing, 50 DEG C of second two is used alternatingly
Alcohol methyl ether acetate and 50 DEG C of dimethyl sulfoxide respectively clean 3 times, and each dosage is 20mL, are finally dried to obtain dyed cotton and knit
Object.
Embodiment 5
By dye composition, 10% formula shown in dye composition shown in 65% formula (I-1), 25% formula (II-1)
(III-1) dye composition shown in mixes active black dye composition.Active black dye composition is dissolved in volume
Dye bath is obtained in anhydrous solvent than ethylene glycol monomethyl ether acetate and dimethyl sulfoxide for 70:30.Then by triethylene diamine
Anhydrous dye bath is added；Additional amount is 6g/L.Ultrasound obtains uniform anhydrous dye bath.Dimethyl sulfoxide swelling and swellbility will be first passed through in advance
It is put into anhydrous dye bath for 22% cotton fabric.Cotton fabric and the bath raio of anhydrous dye bath are 1:16g/mL.Dye dosage is
4o.w.f%.It heats up according to the rate of 3 DEG C/min, is kept the temperature after reaching 85 DEG C of target temperature, dye 5h；It is cooled to after dyeing
Room temperature is used alternatingly 50 DEG C of ethylene glycol monomethyl ether acetate and 50 DEG C of dimethyl sulfoxide and respectively cleans 3 times, and each dosage is
20mL is finally dried to obtain dyed cotton fabric.
Embodiment 6
By dye composition, 10% formula shown in dye composition shown in 65% formula (I-1), 25% formula (II-1)
(III-1) dye composition shown in mixes active black dye composition.Active black dye composition is dissolved in volume
Dye bath is obtained in anhydrous solvent than ethylene glycol monomethyl ether acetate and dimethyl sulfoxide for 70:30.Then tetramethylguanidine is added
Entering amount is 6g/L.Ultrasound obtains uniform anhydrous dye bath.The cotton fabric that dimethyl sulfoxide swelling will be first passed through in advance and swellbility is 22%
It is put into anhydrous dye bath.Cotton fabric and the bath raio of anhydrous dye bath are 1:16g/mL.Dye dosage is 4o.w.f%.According to 3 DEG C/
The rate of min heats up, and keeps the temperature after reaching 85 DEG C of target temperature, dyes 5h；It is cooled to room temperature after dyeing, is used alternatingly 50 DEG C
Ethylene glycol monomethyl ether acetate and 50 DEG C of dimethyl sulfoxide respectively clean 3 times, each dosage be 20mL, be finally dried to obtain dyeing
Cotton fabric.
Comparative example 1
Active black dye composition is replaced with into dye composition shown in 100% formula (I-1), remaining is the same as embodiment 1.
Comparative example 2
Ethylene glycol monomethyl ether acetate is replaced with into glycol dimethyl ether, remaining is the same as embodiment 1.
Comparative example 3
It is added without fixation alkali, remaining is the same as embodiment 1.
Comparative example 4
Active black dye composition is replaced with into dye composition shown in 100% formula (I-2), water is dissolved in and is made into
The dye bath of 2.5g/L.Dry cotton fabric is directly placed into dye bath.Cotton fabric and the bath raio of dye bath are 1:16g/mL.Dyestuff is used
Amount is 4o.w.f%.15% anhydrous sodium sulphate is added at 30 DEG C and keeps the temperature 60min.Then it is warming up to according to the rate of 3 DEG C/min
60 DEG C, and inhale dye 45min.Then the sodium carbonate progress fixation that total amount is equivalent to 20g/L is added in two batches, fixation total duration is
60min.Fabric after dyeing is taken out, washing, soap boiling 15min in 3g/L soap lye is finally dried to obtain dyed cotton fabric.
According to the Integ value and two kinds of degree of fixation of present invention method measurement embodiment 1-6 and comparative example 1-4 above-mentioned.Knot
Fruit is referring to table 1.
Table 1
According to the colour fastness to rubbing and water-fastness color of present invention method measurement embodiment 1-6 and comparative example 1-4 above-mentioned
Fastness (60 DEG C).As a result referring to table 2.
Table 2
Embodiment 1-3 is related to the synchronous colouring method carried out of upper dye fixation it can be seen from Tables 1 and 2, due to using
Specific reactive dye, anhydrous solvent, fixation alkali, can either realize the effect of high corvinus, while having high colour-fast rate and height
Dyefastness.Embodiment 4 is related to contaminating the colouring method that fixation substep carries out, and this method is suitable with embodiment 1-3 effect.Implement
Example 5-6 uses single fixation alkali, although pitch black degree and dyefastness are slightly less than embodiment 1-4, but still is significantly higher than existing
Water-bath colouring method；In addition, degree of fixation is suitable with the prior art.Comparative example 1 is used to confirm that the Integ value of embodiment 1-6 to increase
The value added synergistic function for being mostly derived from three kinds of dye components of active black dye composition.Comparative example 2 and 3 is respectively used to confirm
Specific solvent and the role in the present invention of fixation alkali.Comparative example 4 represents existing water-bath colouring method.
The foregoing is only a preferred embodiment of the present invention, is not intended to restrict the invention, for the skill of this field
For art personnel, the invention may be variously modified and varied.All within the spirits and principles of the present invention, made any to repair
Change, equivalent replacement, improvement etc., is all included in the scope of protection of the present invention.
Claims (1)
1. the synchronous non-aqueous dyeing method carried out of fixation is contaminated on a kind of high pitch black degree cotton fabric, this method comprises: cotton fabric is set
In anhydrous dye bath, heats up according to the rate of 0.5-5 DEG C/min, kept the temperature after reaching 70-100 DEG C of target temperature, dye 1-12h；
It is cooled to room temperature after dyeing, cleans dyed fabric using anhydrous solvent, be finally dried to obtain dyed cotton fabric；Wherein, institute
It states anhydrous dye bath and is dissolved in anhydrous solvent by reactive dye and obtained, the anhydrous solvent is by ethylene glycol monomethyl ether acetate and non-
Proton polar solvent composition；It is characterized in that, the reactive dye are selected from active black dye composition；The method includes heatings
Organic base is further added in the anhydrous dye bath before starting；
Wherein, the active black dye composition includes dye composition A, is selected from appointing for dye composition shown in formula (I)
It anticipates one or more；
(I)
In formula (I), R1-R4It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y1-Y2It selects each independently
From SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Total weight based on active black dye composition calculates, and the weight percent of dye composition A is 45-85%；
The active black dye composition further includes dye composition B, is selected from any of dye composition shown in formula (II)
It is one or more；
(II)
In formula (II), R5-R8It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y3-Y4It selects each independently
From SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Total weight based on active black dye composition calculates, and the weight percent of dye composition B is 15-35%；
The active black dye composition further includes dye composition C, is selected from any of dye composition shown in formula (III)
It is one or more；
(III)
In formula (III), R9-R10It is each independently selected from H, C1-C4Alkyl, C1-C4Alkoxy and SO3M；Y5Independently selected from
SO2CH=CH2Or SO2CH2CH2OSO3M；M is selected from H, Na or K；
Total weight based on active black dye composition calculates, and the weight percent of dye composition C is 5-18%；
Wherein, the organic base is selected from the mixture of triethylene diamine and tetramethylguanidine；The weight of triethylene diamine and tetramethylguanidine
Amount is than being (1.5-2): 1；The additional amount of the organic base is 2-8g/L；
The aprotic polar solvent is selected from dimethyl sulfoxide；
The volume ratio of ethylene glycol monomethyl ether acetate and dimethyl sulfoxide is (65-75): (35-25)；
The cotton fabric first passes through dimethyl sulfoxide swelling in advance.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5731110A (en) * | 1993-02-02 | 1998-03-24 | Sumitomo Chemical Company, Limited | Photoresist composition for use in color filters |
| CN1576330A (en) * | 2003-06-27 | 2005-02-09 | 东洋油墨制造株式会社 | Nonaqueous ink-jet ink |
| CN101151338A (en) * | 2005-09-26 | 2008-03-26 | 三菱化学株式会社 | Colorant dispersion, coloring resin composition, color filter, and liquid-crystal display device |
| CN103360791A (en) * | 2012-04-10 | 2013-10-23 | 住友化学株式会社 | Colorant dispersion liquid |
| CN103614930A (en) * | 2013-11-22 | 2014-03-05 | 东华大学 | Anhydrous recycling dyeing method of activated dye |
| CN105647281A (en) * | 2015-12-24 | 2016-06-08 | 青岛大方智慧网络科技有限公司 | Washable watercolor pen |
-
2018
- 2018-11-19 CN CN201811373624.2A patent/CN109403099B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5731110A (en) * | 1993-02-02 | 1998-03-24 | Sumitomo Chemical Company, Limited | Photoresist composition for use in color filters |
| CN1576330A (en) * | 2003-06-27 | 2005-02-09 | 东洋油墨制造株式会社 | Nonaqueous ink-jet ink |
| CN101151338A (en) * | 2005-09-26 | 2008-03-26 | 三菱化学株式会社 | Colorant dispersion, coloring resin composition, color filter, and liquid-crystal display device |
| CN103360791A (en) * | 2012-04-10 | 2013-10-23 | 住友化学株式会社 | Colorant dispersion liquid |
| CN103614930A (en) * | 2013-11-22 | 2014-03-05 | 东华大学 | Anhydrous recycling dyeing method of activated dye |
| CN105647281A (en) * | 2015-12-24 | 2016-06-08 | 青岛大方智慧网络科技有限公司 | Washable watercolor pen |
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Denomination of invention: Anhydrous dyeing method with simultaneous dyeing and fixation of high black cotton fabric Effective date of registration: 20220725 Granted publication date: 20191122 Pledgee: Zhejiang Shaoxing Ruifeng Rural Commercial Bank Co.,Ltd. Anchang sub branch Pledgor: ZHEJIANG YUEXIN DYEING & PRINTING CO.,LTD. Registration number: Y2022980011137 |