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CN118704252B - A dark dyeing process for water-saving cotton fabric - Google Patents

A dark dyeing process for water-saving cotton fabric Download PDF

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Publication number
CN118704252B
CN118704252B CN202410705121.XA CN202410705121A CN118704252B CN 118704252 B CN118704252 B CN 118704252B CN 202410705121 A CN202410705121 A CN 202410705121A CN 118704252 B CN118704252 B CN 118704252B
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cotton fabric
dyeing
water
modified
hours
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CN118704252A (en
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金京
周四丽
龙涛
马葱葱
李孟三
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Zhejiang Yingfeng Technology Co ltd
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Zhejiang Yingfeng Technology Co ltd
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    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P3/00Special processes of dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form, classified according to the material treated
    • D06P3/58Material containing hydroxyl groups
    • D06P3/60Natural or regenerated cellulose
    • D06P3/66Natural or regenerated cellulose using reactive dyes
    • CCHEMISTRY; METALLURGY
    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/14Methyl esters, e.g. methyl (meth)acrylate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/12Esters of monohydric alcohols or phenols
    • C08F220/16Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms
    • C08F220/18Esters of monohydric alcohols or phenols of phenols or of alcohols containing two or more carbon atoms with acrylic or methacrylic acids
    • C08F220/1804C4-(meth)acrylate, e.g. butyl (meth)acrylate, isobutyl (meth)acrylate or tert-butyl (meth)acrylate
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    • C08ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08FMACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
    • C08F220/00Copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and only one being terminated by only one carboxyl radical or a salt, anhydride ester, amide, imide or nitrile thereof
    • C08F220/02Monocarboxylic acids having less than ten carbon atoms; Derivatives thereof
    • C08F220/10Esters
    • C08F220/34Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate
    • C08F220/343Esters containing nitrogen, e.g. N,N-dimethylaminoethyl (meth)acrylate in the form of urethane links
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    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B67/00Influencing the physical, e.g. the dyeing or printing properties of dyestuffs without chemical reactions, e.g. by treating with solvents grinding or grinding assistants, coating of pigments or dyes; Process features in the making of dyestuff preparations; Dyestuff preparations of a special physical nature, e.g. tablets, films
    • C09B67/0071Process features in the making of dyestuff preparations; Dehydrating agents; Dispersing agents; Dustfree compositions
    • C09B67/0072Preparations with anionic dyes or reactive dyes
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    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09BORGANIC DYES OR CLOSELY-RELATED COMPOUNDS FOR PRODUCING DYES, e.g. PIGMENTS; MORDANTS; LAKES
    • C09B68/00Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology
    • C09B68/40Organic pigments surface-modified by grafting, e.g. by establishing covalent or complex bonds, in order to improve the pigment properties, e.g. dispersibility or rheology characterised by the chemical nature of the attached groups
    • C09B68/42Ionic groups, e.g. free acid
    • C09B68/423Cationic groups
    • C09B68/4235Ammonium groups or derivatives thereof
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    • D06MTREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
    • D06M11/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
    • D06M11/32Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
    • D06M11/36Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with oxides, hydroxides or mixed oxides; with salts derived from anions with an amphoteric element-oxygen bond
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    • D06M13/00Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment
    • D06M13/10Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with non-macromolecular organic compounds; Such treatment combined with mechanical treatment with compounds containing oxygen
    • D06M13/184Carboxylic acids; Anhydrides, halides or salts thereof
    • D06M13/207Substituted carboxylic acids, e.g. by hydroxy or keto groups; Anhydrides, halides or salts thereof
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    • D06M15/00Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
    • D06M15/19Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
    • D06M15/21Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D06M15/263Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof
    • D06M15/267Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of unsaturated carboxylic acids; Salts or esters thereof of unsaturated carboxylic esters having amino or quaternary ammonium groups
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    • D06M16/00Biochemical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. enzymatic
    • DTEXTILES; PAPER
    • D06TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
    • D06PDYEING OR PRINTING TEXTILES; DYEING LEATHER, FURS OR SOLID MACROMOLECULAR SUBSTANCES IN ANY FORM
    • D06P1/00General 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
    • D06P1/38General 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
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    • D06P1/44General 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
    • D06P1/52General 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 synthetic macromolecular substances
    • D06P1/5207Macromolecular compounds obtained by reactions involving only carbon-to-carbon unsaturated bonds
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    • D06P1/90General 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
    • D06P1/92General 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
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    • D06P5/00Other features in dyeing or printing textiles, or dyeing leather, furs, or solid macromolecular substances in any form
    • D06P5/22Effecting variation of dye affinity on textile material by chemical means that react with the fibre
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    • D06M2101/00Chemical constitution of the fibres, threads, yarns, fabrics or fibrous goods made from such materials, to be treated
    • D06M2101/02Natural fibres, other than mineral fibres
    • D06M2101/04Vegetal fibres
    • D06M2101/06Vegetal fibres cellulosic

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Abstract

The invention relates to the field of textile printing and dyeing, and discloses a water-saving cotton fabric dark dyeing process which comprises the steps of taking cotton fabric for modification treatment to obtain modified cotton fabric, soaking the modified cotton fabric in deionized water, wherein the dosage of modified reactive dye is 1-3% (owf), the bath ratio is 1:20-40, the volume fraction of ethanol is 80-90%, dyeing is carried out at room temperature, the temperature rising rate of 2-5 ℃ per minute is increased to 40-60 ℃, dyeing is carried out for 1-2 hours, alkali is added, the temperature rising rate is increased to 60-90 ℃, fixation is carried out for 20-50 minutes, then the temperature reducing rate of 2-5 ℃ per minute is reduced to 30-40 ℃, dyeing is finished, washing, soaping and drying are carried out.

Description

Water-saving cotton fabric dark dyeing process
Technical Field
The invention belongs to the technical field of textile printing and dyeing, and particularly relates to a water-saving cotton fabric deep color dyeing process.
Background
The cotton fabric is concerned by people because of the characteristics of good hydrophilicity, air permeability, softness and the like, and the consumption of the reactive dye serving as the main dye for dyeing the cotton fabric is greatly increased. The reactive dye is usually water as a medium, and because the reactive dye generally has lower substantivity and lower dye uptake, a large amount of neutral electrolyte is needed to be added to promote dyeing in the dyeing process, the dye uptake of the dye is improved, the waste of the dye is reduced, but a large amount of inorganic salt in the wastewater cannot be automatically degraded and is difficult to recover, so that the wastewater treatment difficulty is increased, and the environment is polluted by the discharge of sewage. On the other hand, the water consumption of the water bath dyeing of the reactive dye is large, so that a part of dye is hydrolyzed, the fixation rate is reduced, meanwhile, partial hydrolyzed dye exists in the dyeing wastewater, the water source is seriously polluted, the discharge of the dyeing wastewater brings a plurality of ecological problems, and along with the increasing shortage of water resources and the enhancement of environmental awareness of people, the salt-free and water-free dyeing of the reactive dye gradually becomes an important direction of the research of dyeing technology.
Disclosure of Invention
In order to solve the defects in the background art, the invention aims to provide a water-saving cotton fabric dark dyeing process, which improves the dyeing performance of cotton fabrics and uniformly dyes by modifying cotton fabrics and reactive dyes, and simultaneously adopts an ethanol/water mixed solvent as a system for dyeing cotton fabrics by the reactive dyes, so that the water consumption is reduced, the reactive dyes dye the cotton fabrics under the salt-free condition, and the discharge of dyeing wastewater is reduced.
The aim of the invention can be achieved by the following technical scheme:
The deep dyeing process of the water-saving cotton fabric comprises the following steps of:
S1, modifying cotton fabric to obtain modified cotton fabric;
S2, soaking the modified cotton fabric with deionized water, wherein the dosage of the modified reactive dye is 1-3% (owf), the bath ratio is 1:20-40, and the volume fraction of ethanol is 80-90%;
S3, entering dyeing at room temperature, heating to 40-60 ℃ at a heating rate of 2-5 ℃ per minute, dyeing for 1-2 hours, adding alkali, heating to 60-90 ℃ for fixation for 20-50 minutes, then cooling to 30-40 ℃ at a cooling rate of 2-5 ℃ per minute, finishing dyeing, washing, soaping and drying.
Preferably, the preparation method of the modified cotton fabric in the step S1 includes the following steps:
(1) Putting the cotton fabric into an alkali solution with a bath ratio of 1:50, wherein the mass fraction of sodium hydroxide is 20%, the volume fraction of ethanol is 40%, stirring at 50-70 ℃ for 1-2 hours, and then fully washing and drying to obtain an alkalized cotton fabric;
(2) Soaking the alkalized cotton fabric into a modifier solution with the bath ratio of 1:50, wherein the mass fraction of sodium chloroacetate is 20% and the volume fraction of ethanol is 40%, stirring at 50-70 ℃ for 1-2 hours, washing and drying after the reaction is finished, and neutralizing the excessive alkali on the cotton fabric by using an acetic acid solution to obtain the modified cotton fabric.
Preferably, the preparation method of the modified reactive dye in the step S2 comprises the following steps:
A. Adding 2-hydroxymethyl pyridine and 1-bromotetradecane into a reactor containing a1, 4-dioxane solvent, stirring and reacting at 95-110 ℃ for 36-48 hours, and performing rotary evaporation, washing, suction filtration and drying after the reaction is completed to obtain a quaternary ammonium salt intermediate;
B. Taking a quaternary ammonium salt intermediate, a catalyst dibutyl tin dilaurate, a polymerization inhibitor hydroquinone and anhydrous methylene dichloride, placing the materials in a reactor, stirring and dissolving the materials at 30-35 ℃, then heating the materials to 40-55 ℃, adding isocyano ethyl methacrylate, stirring and reacting the materials for 4-8 hours, and performing rotary evaporation, washing and drying after the reaction is completed to obtain the quaternary ammonium salt cation modifier;
C. adding a quaternary ammonium salt cationic modifier into a reactor filled with deionized water, adding methyl methacrylate and butyl acrylate in a nitrogen atmosphere, stirring and reacting for 1-2 hours, heating to 75-90 ℃, preserving heat for 5-10 minutes, then dropwise adding an azo diisobutyl amidine hydrochloride solution for reacting for 4-6 hours, and cooling and suction filtering after the reaction is completed to obtain cationic microsphere dispersion;
D. And (3) putting the reactive dye into a reactor, slowly dropwise adding the cationic microsphere dispersion liquid into a water bath kettle at the temperature of 25-30 ℃ for 1-1.5 h, stirring for 5-10 min after the dropwise adding, then regulating the pH value of a dye bath to 4-5 by using hydrochloric acid, heating to 60-70 ℃ for dyeing for 2-3 h, and cooling to room temperature after the reaction is completed to obtain the modified reactive dye.
Preferably, in the step A, the mass ratio of the 2-hydroxymethyl pyridine to the 1-bromotetradecane is 1:5-5.5.
Preferably, in the step B, the mass ratio of the quaternary ammonium salt intermediate to the isocyano ethyl methacrylate is 2-3:1.
Preferably, in the step C, the mass ratio of the quaternary ammonium salt cationic modifier, the methyl methacrylate and the butyl acrylate is 5-10:1-4:1.
Preferably, the concentration of the cationic microsphere dispersion liquid in the step D is 1-2 g/L, and the mass ratio of the reactive dye to the cationic microsphere dispersion liquid is 0.08-1.2:1.
Preferably, the reactive dye is any one of c.i. reactive red 195, c.i. reactive yellow 95, c.i. reactive blue 72.
The invention has the beneficial effects that:
The invention utilizes 2-hydroxymethyl pyridine to react with 1-bromotetradecane to synthesize a quaternary ammonium salt intermediate, then reacts with isocyanoethyl methacrylate to synthesize a quaternary ammonium salt cationic modifier containing a double bond structure, the quaternary ammonium salt cationic modifier, methyl methacrylate and butyl acrylate are mixed, azo diisobutyl amidine hydrochloride is used as an initiator, and methyl methacrylate, butyl acrylate and the quaternary ammonium salt cationic modifier are initiated to copolymerize in a water phase to synthesize the cationic polymer microsphere. The methyl methacrylate and butyl acrylate are nonionic monomers, the butyl acrylate can improve the polymerization reaction rate to induce the formation of polymer microspheres, meanwhile, the synthetic cationic polymer microspheres are stabilized to a certain extent, the quaternary ammonium salt cationic modifier is a cationic monomer, quaternary ammonium salt functional groups in the structure enable the surfaces of the cationic polymer microspheres to be positively charged, and meanwhile, the quaternary ammonium salt functional groups have broad-spectrum antibacterial effect and can endow cotton fabrics with good antibacterial effects. The invention uses reactive dye to dye cationic polymer microsphere, the reactive dye can ionize in aqueous solution to generate sulfonic group and has negative charge, the surface of the cationic polymer microsphere has positive charge due to quaternary ammonium salt group, and the reactive dye approaches to the cationic polymer microsphere due to electrostatic attraction, hydrogen bond and Van der Waals force, and is adsorbed on the microsphere surface to prepare the modified reactive dye.
According to the invention, the cotton fabric is subjected to alkalization treatment to remove impurities, so that the surface of the cotton fabric is smoother, and then is treated by sodium chloroacetate, carboxyl ions are loaded on the cotton fabric, so that the cotton fabric is anionized, the charging performance of the cotton fabric can be changed, the dyeing depth of the modified reactive dye on the cotton fabric can be improved, the anionized cotton fabric is dyed by using the modified reactive dye, the defect that the reactive dye can only be directly combined with the cotton fabric by hydrogen bonds or Van der Waals force is overcome, the cationic polymer microspheres are combined with the modified cotton fabric in a covalent bond/ionic bond manner, the application effect of the cationic polymer microspheres on the cotton fabric is enhanced, in addition, the cationic polymer microspheres have large specific surface area and uniform size, the reflectivity of the cotton fabric surface to light is reduced, the light absorption capacity of the fabric surface is increased, the dyed cotton fabric is deepened, and the utilization rate of the reactive dye is effectively improved. The invention uses the reactive dye to dye the cationic polymer microsphere, then uses the cationic polymer microsphere with positive charge and the cotton fabric with negative charge to combine, and does not need to add salt to promote dyeing as in the traditional process, and adopts the salt-free and water-free dyeing process. The invention adopts the ethanol/water mixed solvent as a system for dyeing cotton fabrics by using the reactive dye, reduces the water consumption, enables the reactive dye to dye the cotton fabrics under the salt-free condition, further reduces the discharge of dyeing wastewater, and enables the ethanol to be recycled after dyeing, thereby being an environment-friendly dyeing method.
Detailed Description
The technical solutions of the embodiments of the present invention will be clearly and completely described below in conjunction with the embodiments of the present invention, and it is apparent that the described embodiments are only some embodiments of the present invention, not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
The cotton fabrics of the examples and comparative examples of the present invention were 100% pure cotton plain weave, 133g/m 2, produced by well known bright textile Co., ltd, and C.I. reactive red 195, produced by Shanghai Anno group Co., ltd.
Example 1a method of making a modified cotton fabric includes the steps of:
(1) Putting cotton fabric into alkali solution with bath ratio of 1:50, wherein the mass fraction of sodium hydroxide is 20%, the volume fraction of ethanol is 40%, stirring at 60 ℃ for 1h, and then fully washing and drying to obtain alkalized cotton fabric:
(2) Soaking the alkalized cotton fabric into a modifier solution with the bath ratio of 1:50, wherein the mass fraction of sodium chloroacetate is 20%, the volume fraction of ethanol is 40%, stirring at 60 ℃ for 1h, washing and drying after the reaction is finished, and neutralizing the excessive alkali on the cotton fabric by using a 1% acetic acid solution to obtain the modified cotton fabric.
Example 2a process for preparing a modified reactive dye comprises the steps of:
A. Adding 5g of 2-hydroxymethyl pyridine and 25.7g of 1-bromotetradecane into a reactor containing 200ml of 1, 4-dioxane solvent, stirring and reacting for 48 hours at 105 ℃, and performing rotary evaporation, washing, suction filtration and drying after the reaction is finished to obtain a quaternary ammonium salt intermediate;
B. Taking 5g of quaternary ammonium salt intermediate, 0.002g of catalyst dibutyl tin dilaurate, 0.03g of polymerization inhibitor hydroquinone and 100mL of anhydrous dichloromethane, placing the materials in a reactor, stirring and dissolving at 30 ℃, then heating to 40 ℃, adding 2g of isocyano ethyl methacrylate, stirring and reacting for 6 hours, and performing rotary evaporation, washing and drying after the reaction is completed to obtain the quaternary ammonium salt cation modifier;
C. Adding 5g of quaternary ammonium salt cationic modifier into a reactor filled with 100mL of deionized water, adding 4g of methyl methacrylate and 1g of butyl acrylate in a nitrogen atmosphere, stirring and reacting for 2h, heating to 85 ℃, preserving heat for 5min, then dropwise adding 10g/L of azo diisobutyl amidine hydrochloride solution for reacting for 6h, and cooling and suction filtering after the reaction is completed to obtain cationic microsphere dispersion;
D. 15mL of active red 195 with the concentration of 0.2g/L is taken and placed in a reactor, 10mL of cationic microsphere dispersion with the concentration of 1g/L is slowly dripped in a water bath kettle with the temperature of 25 ℃ for 1h, the mixture is stirred for 5min after dripping, then hydrochloric acid is used for adjusting the pH value of a dye bath to 5, the temperature is raised to 70 ℃ for dyeing for 2h, and the mixture is cooled to room temperature after the reaction is completed, so as to obtain the modified active dye.
Embodiment 3a water-saving cotton fabric dark dyeing process comprises the following steps:
S1, soaking 3g of modified cotton fabric with deionized water, wherein the dosage of modified reactive dye is 1% (owf), the bath ratio is 1:20, and the volume fraction of ethanol is 80%;
S2, dyeing at room temperature, namely heating to 40 ℃ at a heating rate of 2 ℃ per minute, dyeing for 2 hours, adding 2g/L sodium hydroxide, heating to 60 ℃, fixing color for 30 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Embodiment 4a water-saving cotton fabric dark dyeing process comprises the following steps:
s1, soaking 3g of modified cotton fabric with deionized water, wherein the dosage of modified reactive dye is 2% (owf), the bath ratio is 1:30, and the volume fraction of ethanol is 90%;
S2, dyeing at room temperature, namely heating to 50 ℃ at a heating rate of 5 ℃ per minute, dyeing for 1h, adding 2g/L sodium hydroxide, heating to 70 ℃, fixing color for 50 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Embodiment 5a water-saving cotton fabric dark dyeing process, comprising the following steps:
s1, soaking 3g of modified cotton fabric with deionized water, wherein the dosage of modified reactive dye is 3% (owf), the bath ratio is 1:40, and the volume fraction of ethanol is 90%;
S2, dyeing at room temperature, namely heating to 60 ℃ at a heating rate of 2 ℃ per minute, dyeing for 2 hours, adding 2g/L sodium hydroxide, heating to 80 ℃, fixing color for 30 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Comparative example 1a water-saving cotton fabric dark dyeing process comprising the following steps:
s1, soaking 3g of cotton fabric with deionized water, wherein the dosage of modified reactive dye is 1% (owf), the bath ratio is 1:20, and the volume fraction of ethanol is 80%;
S2, dyeing at room temperature, namely heating to 40 ℃ at a heating rate of 2 ℃ per minute, dyeing for 2 hours, adding 2g/L sodium hydroxide, heating to 60 ℃, fixing color for 30 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Comparative example 2a water-saving cotton fabric dark dyeing process comprising the steps of:
s1, soaking 3g of modified cotton fabric with deionized water, wherein the dosage of active red 195 is 1% (owf), the bath ratio is 1:20, and the volume fraction of ethanol is 80%;
S2, dyeing at room temperature, namely heating to 40 ℃ at a heating rate of 2 ℃ per minute, dyeing for 2 hours, adding 2g/L sodium hydroxide, heating to 60 ℃, fixing color for 30 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Comparative example 3a water-saving cotton fabric dark dyeing process comprising the steps of:
s1, soaking 3g of cotton fabric with deionized water, wherein the dosage of active red 195 is 1% (owf), the bath ratio is 1:20, adding water-soluble dye, and then adding 30g/L sodium chloride;
S2, dyeing at room temperature, namely heating to 40 ℃ at a heating rate of 2 ℃ per minute, dyeing for 2 hours, adding 2g/L sodium hydroxide, heating to 60 ℃, fixing color for 30 minutes, cooling to 30 ℃ at a cooling rate of 5 ℃ per minute, and washing, soaping and drying.
Performance detection
Performance testing of the cotton fabrics prepared in examples 3-5 and comparative examples 1-3:
(1) K/S test is calculated by using a Kubelka-Monk function K/S= (1-R) 2/2R. Wherein K is the absorption coefficient of the fabric to be tested, S is the scattering coefficient of the fabric to be tested, and R is the inversion rate of the fabric to be tested at the maximum absorption wavelength. And measuring the K/S value of the dyed fabric at the maximum absorption wavelength by using a color measuring and matching instrument. The larger the K/S value, the darker the color, and the smaller the K/S value, the lighter the color. Each sample was tested 4 times at different sites and averaged to give the data results shown in table 1.
(2) The percentage of dye uptake was measured by an ultraviolet-visible spectrophotometer and the absorbance of the dye liquor before and after dyeing was calculated to give percentage of dye uptake= (1-nA 1/mA0). Times.100%, wherein A 0 was absorbance of the dye liquor before dyeing diluted m-fold, and A 1 was absorbance of the residual liquor after dyeing diluted n-fold, and the data were shown in Table 1.
(3) Color fastness testing the rubbing fastness of the dyed cotton fabric was measured using a rubbing color fastness tester according to GB/T3920-2008 "textile color fastness test", and the soaping fastness of the dyed cotton fabric was measured using a soaping fastness tester according to GB/T3921-2008 "textile color fastness test", with the data results shown in Table 1.
(4) Leveling test the leveling of the fabric was assessed according to the standard deviation of apparent colour depth between different test sites of the same dyed fabric. The standard deviation of the K/S values was calculated for each of the 8 randomly selected test sites on the dyed fabric, and the data results are shown in Table 1.
TABLE 1 sample Performance test results
As can be seen from the data in Table 1, the cotton fabrics prepared in examples 3 to 5 of the present invention have good dyeing properties, are uniformly dyed, have color fastness in ethanol/water systems and cotton staining fastness reaching 4 to 5 levels, have dry rubbing fastness and wet rubbing fastness reaching 4 to 5 levels, are not obviously different from the water bath dyeing in comparative example 3, and have excellent color fastness at all levels. Wherein the cotton fabric is not modified in comparative example 1, the reactive dye is not modified in comparative example 2, and the dyeing properties of the cotton fabrics prepared in comparative examples 1 to 3 are all inferior to those of examples 3 to 5.
In the description of the present specification, the descriptions of the terms "one embodiment," "example," "specific example," and the like, mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the present invention. In this specification, schematic representations of the above terms do not necessarily refer to the same embodiments or examples. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The foregoing has shown and described the basic principles, principal features and advantages of the invention. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, and that the above embodiments and descriptions are merely illustrative of the principles of the present invention, and various changes and modifications may be made without departing from the spirit and scope of the invention, which is defined in the appended claims.

Claims (6)

1. The deep dyeing process of the water-saving cotton fabric is characterized by comprising the following steps of:
S1, modifying cotton fabric to obtain modified cotton fabric;
S2, soaking the modified cotton fabric with deionized water, wherein the dosage of the modified reactive dye is 1-3%, the bath ratio is 1:20-40, and the volume fraction of ethanol is 80-90%;
S3, entering a dyeing process at room temperature, heating to 40-60 ℃ at a heating rate of 2-5 ℃ per minute, dyeing for 1-2 hours, adding alkali, heating to 60-90 ℃ for fixation for 20-50 minutes, then cooling to 30-40 ℃ at a cooling rate of 2-5 ℃ per minute, finishing dyeing, washing, soaping and drying;
The preparation method of the modified cotton fabric in the step S1 comprises the following steps:
(1) Putting the cotton fabric into an alkali solution with a bath ratio of 1:50, wherein the mass fraction of sodium hydroxide is 20%, the volume fraction of ethanol is 40%, stirring at 50-70 ℃ for 1-2 hours, and then fully washing and drying to obtain an alkalized cotton fabric;
(2) Soaking the alkalized cotton fabric into a modifier solution with a bath ratio of 1:50, wherein the mass fraction of sodium chloroacetate is 20% and the volume fraction of ethanol is 40%, stirring at 50-70 ℃ for 1-2 hours, washing and drying after the reaction is completed, and neutralizing excessive alkali on the cotton fabric by using an acetic acid solution to obtain the modified cotton fabric;
The preparation method of the modified reactive dye in the step S2 comprises the following steps:
A. Adding 2-hydroxymethyl pyridine and 1-bromotetradecane into a reactor containing a1, 4-dioxane solvent, stirring and reacting at 95-110 ℃ for 36-48 hours, and performing rotary evaporation, washing, suction filtration and drying after the reaction is completed to obtain a quaternary ammonium salt intermediate;
B. Taking a quaternary ammonium salt intermediate, a catalyst dibutyl tin dilaurate, a polymerization inhibitor hydroquinone and anhydrous methylene dichloride, placing the materials in a reactor, stirring and dissolving the materials at 30-35 ℃, then heating the materials to 40-55 ℃, adding isocyano ethyl methacrylate, stirring and reacting the materials for 4-8 hours, and performing rotary evaporation, washing and drying after the reaction is completed to obtain the quaternary ammonium salt cation modifier;
C. adding a quaternary ammonium salt cationic modifier into a reactor filled with deionized water, adding methyl methacrylate and butyl acrylate in a nitrogen atmosphere, stirring and reacting for 1-2 hours, heating to 75-90 ℃, preserving heat for 5-10 minutes, then dropwise adding an azo diisobutyl amidine hydrochloride solution for reacting for 4-6 hours, and cooling and suction filtering after the reaction is completed to obtain cationic microsphere dispersion;
D. And (3) putting the reactive dye into a reactor, slowly dropwise adding the cationic microsphere dispersion liquid into a water bath kettle at the temperature of 25-30 ℃ for 1-1.5 h, stirring for 5-10 min after the dropwise adding, then regulating the pH value of a dye bath to 4-5 by using hydrochloric acid, heating to 60-70 ℃ for dyeing for 2-3 h, and cooling to room temperature after the reaction is completed to obtain the modified reactive dye.
2. The water-saving cotton fabric dark dyeing process according to claim 1, wherein the mass ratio of the 2-hydroxymethyl pyridine to the 1-bromotetradecane in the step A is 1:5-5.5.
3. The water-saving cotton fabric dark dyeing process according to claim 1, wherein the mass ratio of the quaternary ammonium salt intermediate to the isocyano ethyl methacrylate in the step B is 2-3:1.
4. The water-saving cotton fabric dark dyeing process according to claim 1, wherein the mass ratio of the quaternary ammonium salt cationic modifier to the methyl methacrylate to the butyl acrylate in the step C is 5-10:1-4:1.
5. The water-saving cotton fabric dark dyeing process according to claim 1, wherein the concentration of the cationic microsphere dispersion liquid in the step D is 1-2 g/L, and the mass ratio of the reactive dye to the cationic microsphere dispersion liquid is 0.08-1.2:1.
6. The process for dark dyeing of water-saving cotton fabric according to claim 1, wherein the reactive dye is any one of c.i. reactive red 195, c.i. reactive yellow 95 and c.i. reactive blue 72.
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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104514158A (en) * 2013-09-26 2015-04-15 五邑大学 Chitosan quaternary ammonium salt for salt-free dyeing of reactive dye and preparation method thereof
CN109322176A (en) * 2018-09-15 2019-02-12 杭州三印染整有限公司 A kind of cotton-polyester blend fabric dye composite and its colouring method

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CN115162033B (en) * 2022-05-13 2024-07-16 东华大学 Low-resource-consumption salt-free low-alkali reactive dye dyeing method

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104514158A (en) * 2013-09-26 2015-04-15 五邑大学 Chitosan quaternary ammonium salt for salt-free dyeing of reactive dye and preparation method thereof
CN109322176A (en) * 2018-09-15 2019-02-12 杭州三印染整有限公司 A kind of cotton-polyester blend fabric dye composite and its colouring method

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