A non-aqueous medium dyeing process for disperse reactive dyes with variable affinity

Abstract

The invention relates to a non-aqueous medium dyeing process of disperse active dyes with convertible affinity, wherein wet fabric or yarn is placed in a disperse active dye solution for dyeing to obtain the dyed fabric or yarn; the wet fabric or yarn is obtained by placing a cellulose fiber fabric or yarn in an alkaline solution with a pH value of 7.5-11 for swelling; the disperse active dye solution is a solution obtained by dissolving disperse active dyes with convertible affinity in a weak polar or non-polar solvent with a relative dielectric constant of less than 5; the disperse active dyes with convertible affinity are disperse active dyes containing both a group with convertible affinity and an active group in the molecular structure, and under an alkaline condition of a pH value of 7.5-11, the reaction activity of the group with convertible affinity with water is greater than the reaction activity of the active group with cellulose; the method of the invention ensures that the cellulose fiber has high dye uptake and fixation rates, and has excellent level dyeing and dyeing depth, and good fastness in various aspects.

Description

Technical Field

[0001] The invention belongs to the technical field of dyeing and relates to a non-aqueous medium dyeing process of disperse active dyes with convertible affinity. Background Art

[0002] In the non-aqueous medium reactive dye dyeing of cellulose fibers, a weak polar solvent (or non-polar solvent) is added as a mass transfer medium, and a trace amount of water (or other polar solvents) is added to swell the fibers and provide an alkaline reaction environment; however, weak polar solvents (or non-polar solvents) have poor solubility for reactive dyes, so reactive dyes are present in trace amounts of water (or other polar solvents), which leads to two problems:

[0003] (1) The concentration of dye in trace water (or other polar solvents) is high, which affects its diffusion into the fiber and easily causes problems such as color spots and color flowers;

[0004] (2) When dyeing, the dye concentration is too high and the dye aggregates are large. After dyeing, large aggregates are easily induced to cause aggregation-induced visible light quenching, making the color of the dyed product dark.

[0005] In the scheme provided by patent CN201910004467.6, cotton fabric is first immersed in alkali solution in advance, taken out, and then the reactive dye aqueous solution is dispersed in the non-aqueous medium anisole to prepare a mixed emulsion of anisole and dye solution, and then the cotton fabric is dyed by the process of immersion dyeing; the organic solvent after dyeing can be recovered by centrifugal separation, saving water and energy, and reducing sewage discharge. The water washing fastness can reach level 4, and the dry and wet friction fastness can reach levels 3.5 and 3; however, this method does not solve the above two problems.

[0006] Reference 1 (Reactive dye dyeing of cotton fabrics in ethanol-water system and related theoretical research [D]. Donghua University, 2014.) provides a scheme in which no salt is needed when dyeing in an ethanol / water system (ethanol with a volume fraction of 80%). When the amount of alkali used is 1 / 10 of that in traditional dyeing, the dye uptake rate is 97%, and the fixation rate is 9% to 20% higher than that in traditional dyeing, saving 30.5% to 42.5% of dyes while having good color fastness. However, the ethanol / water system has a high selectivity for reactive dyes. Only reactive dyes that are insoluble in ethanol can obtain a high dye uptake rate and fixation rate. Dyes that are soluble in ethanol cannot be dyed even if salt and alkali are added to promote dyeing. At the same time, the above two problems are not solved.

[0007] In view of the above problems, there are mainly three solutions in the prior art, which are as follows:

[0008] Solution 1: Use high temperature (above 100°C) to intensify the movement of dye molecules, making the diffusion process easier and the degree of aggregation weaker. However, high temperature first leads to high energy consumption, and secondly, it may cause fiber damage and reduced strength. As provided in the solution of patent CN201610177603.8, cotton fabric is immersed in sodium carbonate aqueous solution for swelling, the liquid rate is controlled, and it is placed in a dimethyl sulfoxide solution containing active dyes for dyeing. Tetrachloroethylene is slowly added during the heating process, and the temperature is raised to 130°C for 2h. Take out the dyed cloth sample, dry and recover the solvent, and then evenly atomize 30g / L of the color fixing agent SENKAFIXSCF-88 to form droplets of 30-70μm, and then evenly spray the droplets on both sides of the cloth sample, control the liquid rate, and dry at 70-80°C for 3-10min to complete dyeing and fixation. After dyeing, the dyeing rate can reach 100%, the color fixation rate can reach 99.9%, and the color fastness to washing can reach level 4.5. The dry and wet friction fastness can reach 4.0 and 2.5. However, this method takes too long to dye and the dyeing temperature is high. High temperature will lead to high energy consumption. Secondly, it will cause certain damage to the mechanical properties of the fiber. The fiber will be damaged and the strength will decrease. Finally, the dimethyl sulfoxide used in the process is toxic and has a strong odor. The residual cloth surface is harmful to the human body and the solvent recovery is troublesome.

[0009] Solution 2: Use a dispersant to suspend the active dye solution in a weak polar solvent in the form of micro-droplets to prevent excessive aggregation of the dye. However, after dyeing is completed, the separation and treatment of the residual dispersant and dye in the solvent, as well as the recovery of the solvent, are difficult to solve. For example, in Reference 2 (Investigating the Effect of Dispersants on the Dyeing Performance of Disperse Dyes in Silicon-based Non-aqueous Media [D]. Zhejiang Sci-Tech University, 2021.), a dispersant is used to disperse the active dye in the D5 solvent, and the dye is dyed in the form of a suspension. The cotton fabric is pre-soaked in alkali solution to achieve a high dye uptake and fixation rate and good leveling. This method uses a dispersant to suspend the active dye solution in a weak polar solvent in the form of micro-droplets to prevent excessive aggregation of the dye. Although D5-suspension dyeing has a high dye uptake and fixation rate, it is difficult to control the size of the suspension droplets and the dye concentration therein. At the same time, it is also difficult to separate and recover the dispersant, residual dye and D5 medium after dyeing.

[0010] Solution 3: Use disperse reactive dyes for dyeing. Although it has good solubility in weakly polar solvents, it has poor affinity for water and fibers, resulting in a low dyeing rate. Poor affinity also makes it difficult for the reactive groups of the dye to contact the hydroxyl groups on the cellulose fibers for covalent bond reaction, so the fixation rate is low and the color fastness is poor. For example, in the solution provided in Reference 3 (Novel sustainable synthesis of dyes for clean dyeing of wool and cotton fibres in supercritical carbon dioxide [J]. Journal of Cleaner Production, 2018, 199: 1-10.), in supercritical CO 2 In the fluid, disperse reactive dyes are used to dye cotton, and the cotton fibers need to be swollen and alkalized with a certain amount of alkali solution in advance; in this method, disperse reactive dyes are used for dyeing, and the solubility of disperse reactive dyes in weak polar solvents is relatively good, which solves the problem of high concentration in trace water (or other polar solvents). However, disperse reactive dyes have poor affinity for water and fibers, resulting in a relatively low dyeing rate. Poor affinity also makes it difficult for the reactive groups of the dye to contact the hydroxyl groups on the cellulose fibers for covalent bond reactions, so the color fixation rate is low and the color fastness is poor. Summary of the invention

[0011] In order to solve the problems existing in the prior art, the present invention provides a non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity.

[0012] To achieve the above object, the scheme adopted by the present invention is as follows:

[0013] A non-aqueous dyeing process of disperse active dyes with convertible affinity, wherein wet fabric or yarn is placed in a disperse active dye solution for dyeing, and after soaping and drying, the dyed fabric or yarn is obtained;

[0014] The wet fabric or yarn is obtained by swelling the cellulose fiber fabric or yarn in an alkaline solution with a pH of 7.5 to 11;

[0015] The disperse reactive dye solution is a solution obtained by dissolving a disperse reactive dye with convertible affinity in a weakly polar or non-polar solvent with a relative dielectric constant of less than 5;

[0016] Affinity-convertible disperse reactive dyes are disperse reactive dyes containing both affinity-convertible groups and reactive groups in their molecular structures. Under alkaline conditions of pH 7.5 to 11, the reactivity of the affinity-convertible groups with water is greater than the reactivity of the reactive groups with cellulose.

[0017] As the preferred technical solution:

[0018] In the above-mentioned non-aqueous dyeing process with disperse reactive dyes having convertible affinity, the liquid carrying rate of the wet fabric or yarn is 30-80%.

[0019] In the above-mentioned affinity-changeable disperse reactive dye non-aqueous medium dyeing process, the affinity-changeable group is a fluorosulfonyl group or a sulfonate group, and the active group is a vinyl sulfone type active group, a triazine type active group, a pyrimidine type active group or a carbamate type active group.

[0020] In the above-mentioned non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the weakly polar or non-polar solvent with a relative dielectric constant of less than 5 is isooctane, liquid paraffin, mineral oil, anisole, dimethyl carbonate, silicones, edible oil or supercritical CO 2 fluid.

[0021] The above-mentioned affinity-convertible disperse reactive dye non-aqueous medium dyeing process has a dyeing temperature of 40 to 100° C. and a dyeing time of 0.5 to 2 hours.

[0022] In the above-mentioned affinity-convertible disperse reactive dye non-aqueous medium dyeing process, the bath ratio during dyeing is 1:10-100, and the dye dosage during the dyeing process is 0.1-10% omf.

[0023] In the above-mentioned non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the alkaline solution is one or more of sodium carbonate solution, sodium bicarbonate solution, sodium hydroxide solution, potassium hydroxide solution, sodium silicate solution, sodium phosphate solution, sodium hydrogen phosphate solution and sodium acetate solution.

[0024] In the above-mentioned non-aqueous dyeing process of disperse reactive dyes with variable affinity, the concentration of the alkaline solution is 10 -7 ~10 -2 mol / L.

[0025] In the above-mentioned affinity-convertible disperse reactive dye non-aqueous medium dyeing process, the concentration of the disperse reactive dye solution is 0.01-5 g / L.

[0026] A non-aqueous dyeing process for disperse reactive dyes with variable affinity as described in any of the above items, wherein the dyed fabric or yarn has a color absorption rate greater than 95%, a color fixation rate greater than 90%, a dry rubbing fastness greater than grade 4, a wet rubbing fastness greater than grade 3-4, a color change fastness greater than grade 4, and a cotton staining fastness greater than grade 4-5;

[0027] Take 10 points from the dyed fabric or yarn to measure the LAB value, and the CIELAB color difference between the 10 points is <0.5.

[0028] Principle of the invention:

[0029] In the present invention, the dispersed active dye containing affinity convertible groups has good solubility in weak polar solvents. After the dispersed active dye contacts with water-containing fibers during dyeing, it is hydrolyzed under weak alkaline conditions, and affinity conversion occurs, from originally affinity for weak polar solvents and non-hydrophilicity to non-affinity for weak polar solvents and hydrophilicity. During the dyeing process, the dye gradually transfers from the weak polar solvent to the hydrophilic fiber surface and then dyes the fiber. Under alkaline conditions, the dye undergoes a covalent bond reaction with the hydroxyl group on the fiber to perform color fixation, thereby solving the problem of excessively high dye concentration in trace water caused by the insolubility of the active dye in the weak polar solvent, and also solving the problem of low dye uptake and poor color fixation effect of common dispersed active dyes. In addition, the solvent is non-toxic and easy to recycle.

[0030] The affinity-convertible disperse reactive dye is a disperse reactive dye containing both affinity-convertible groups and reactive groups in its molecular structure; the affinity-convertible group is a fluorosulfonyl group or a sulfonate group, and the reactive group is a vinyl sulfone type reactive group, a triazine type reactive group, a pyrimidine type reactive group or a carbamate type reactive group.

[0031] In the prior art, Document 4 (Synthesis and properties of some novel pyrazolone-based heterocyclic azo disperse dyes containing a fluorosulfonyl group [J]. Dyes and Pigments, 2012, 95 (3): 580-586.) and Document 5 (Synthesis and spectral properties of alkali-clearable azo disperse dyes containing a fluorosulfonyl group [J]. Dyes and pigments, 2003, 56 (1): 69-81.) provide disperse dyes containing a fluorosulfonyl group, which are both used for dyeing synthetic fibers. Such disperse dyes mainly utilize the characteristic of being easily hydrolyzed under alkaline conditions, so that the synthetic fiber products dyed with disperse dyes can remove floating colors by soaping under alkaline conditions, thereby achieving the effect of eliminating reduction cleaning.

[0032] The difference between the present invention and the dye is that the dye is designed to utilize the characteristics of fluorosulfonyl groups, sulfonate groups and other groups that are easily hydrolyzed under weak alkaline conditions, so that its affinity for solvents is changed from the original non-ionic dye that is affinity for weak polar solvents to a hydrophilic ionic dye. In addition, the dye also has an active group that can react with cellulose, so that the dye can gradually dye cellulose fibers in a non-aqueous medium and be fixed in the form of covalent bonds, thereby solving the problems of difficult dye diffusion, color spots and dimming in the non-aqueous medium dyeing process.

[0033] In the prior art, document 6 (Dyeing properties of a reactive disperse dye carrying acetoxyethylsulphone group [J]. Dyes and pigments, 2007, 75 (1): 170-175.) provides disperse reactive dyes containing vinyl sulfone acetate reactive groups for dyeing nylon and polyester blended fibers. After the vinyl sulfone acetate groups are hydrolyzed, they are still water-insoluble dyes without affinity conversion effects. If used for dyeing cellulose fibers such as cotton, there are still problems of low dye uptake and fixation rates.

[0034] Beneficial Effects

[0035] The method of the present invention can significantly reduce the water consumption and water pollution problems of cellulose fiber dyeing when only a small amount of water is used to swell the fiber, and has excellent levelness and depth of dyeing, bright and vivid color, and good fastness in various aspects while ensuring high dye uptake and fixation rates. DETAILED DESCRIPTION

[0036] The present invention will be further described below in conjunction with specific embodiments. It should be understood that these embodiments are only used to illustrate the present invention and are not intended to limit the scope of the present invention. In addition, it should be understood that after reading the content taught by the present invention, those skilled in the art can make various changes or modifications to the present invention, and these equivalent forms fall within the scope limited by the appended claims of the application equally.

[0037] The test methods involved in the embodiments are as follows:

[0038] Color absorption rate and color fixation rate: Determined according to GB / T 2391-2003 "Determination of color absorption rate and color fixation rate of reactive dyes".

[0039] Rubbing fastness: Determined according to GB / T 3920-2008 “Textiles - Tests for colour fastness - Colour fastness to rubbing”.

[0040] Washing fastness: Determined according to GB / T 2391-2008 “Textiles - Tests for colour fastness - Colour fastness to washing with soap”.

[0041] Color difference calculation: calculated according to GB T 8424.3-2001 "Calculation of color difference in color fastness tests for textiles".

[0042] Example 1

[0043] A method for preparing dye blue A, the specific steps are as follows:

[0044] (1) Preparation of intermediates:

[0045] The preparation method of intermediate A is as follows:

[0046] (a) adding 5 g (16 mmol) of 1,4-diaminoanthraquinone-2-sulfonic acid (CAS 4095-85-6) to 25 mL of chlorosulfonic acid at 0°C, warming the mixture to room temperature within 30 min, stirring for 2 h, adding the reaction mixture to ice water, filtering, washing, and vacuum drying to obtain 1,4-diaminoanthraquinone-2-sulfonyl chloride;

[0047] (b) 2 mL of dichloromethane was added to a reaction vessel, and 0.5 mmol of 1,4-diaminoanthraquinone-2-sulfonyl chloride and 0.5 mmol of ethanol were added together for esterification, and 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine was added for catalytic reaction to obtain an intermediate A.

[0048] The preparation method of intermediate B is as follows:

[0049] (I) adding 5 g (22 mmol) of 2,4,6-trimethyl-3,5-diaminobenzenesulfonic acid (CAS 32432-55-6) to 25 mL of chlorosulfonic acid at 0° C., warming the mixture to room temperature within 30 min, stirring for 2 h, and adding the reaction mixture to ice water to obtain 2,4,6-trimethyl-3,5-diaminobenzenesulfonyl chloride;

[0050] (II) 2 mL of dichloromethane was added to a reaction vessel, and 0.5 mmol of 2,4,6-trimethyl-3,5-diaminobenzenesulfonyl chloride and 0.5 mmol of ethanol were added together for esterification, and 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine was added to catalyze the reaction to obtain an intermediate B.

[0051] (2) Synthesis of dyes, the specific steps are as follows:

[0052] (2.1) adding flake ice to water, stirring, adding an ice-milling aid (the volume percentage of the ice-milling aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-milling the intermediate A for 5 minutes to obtain an ice-milled intermediate A;

[0053] (2.2) Add intermediate B to water, adjust the pH to 4 with sodium carbonate to dissolve intermediate B, and obtain an intermediate B solution;

[0054] (2.3) Cooling the intermediate B solution to 10°C with ice, and then adding it to the intermediate A ground with ice in step (2.1), maintaining the temperature at 5°C and the pH at 3; wherein the molar ratio of intermediate A to intermediate B is 1:1;

[0055] (2.4) The pH of the solution mixed in step (2.3) was adjusted to 3.5 with a baking soda suspension, and the mixture was stirred at 5°C and pH = 3.5 for 4 hours. The product was condensed with 5-chloro-2,4,6-trifluoropyrimidine in a molar ratio of 1:1 to obtain dye blue A.

[0056] The structural formula of the dye blue A obtained is:

[0057] A method for preparing dye Orange B, the specific steps are as follows:

[0058] (1) Preparation of intermediates:

[0059] (1.1) 5 g (13 mmol) of 7-amino-1,3,6-naphthalenetrisulfonic acid (CAS 118-03-6) was added to 25 mL of chlorosulfonic acid at 0°C, the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 7-amino-1,3,6-naphthalenetrisulfonyl chloride;

[0060] (1.2) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 7-amino-1,3,6-naphthalenetrisulfonyl chloride and 1.5 mmol of methanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a diazo component;

[0061] (1.3) Add the diazo component to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11;

[0062] (1.4) Sodium carbonate was added to the diazonium salt solution to adjust the pH to 5, and ureaaniline (Hubei Qifei Pharmaceutical Chemical Co., Ltd., CAS 25711-72-2) was added while maintaining the temperature at 10°C to cause a coupling reaction to obtain an intermediate; wherein the molar ratio of the diazonium salt to the ureaaniline was 1:1.

[0063] (2) Synthesis of dyes, the specific steps are as follows:

[0064] (2.1) Add flake ice to water, stir, add ice grinding aid (the volume percentage composition of the ice grinding aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice grind 1,3,5-trifluoro-s-triazine (Chongqing Ruiya Biotechnology Co., Ltd., CAS 675-14-9) for 5 minutes to obtain ice-milled 1,3,5-trifluoro-s-triazine;

[0065] (2.2) adding the intermediate to water, adjusting the pH to 4 with sodium carbonate to dissolve the intermediate, and obtaining an intermediate solution;

[0066] (2.3) Cooling the intermediate solution to 10° C. with ice, and then adding it to the 1,3,5-trifluoro-s-triazine ground with ice in step (2.1), maintaining the temperature at 5° C. and pH = 3; wherein the molar ratio of the intermediate to 1,3,5-trifluoro-s-triazine is 1:1;

[0067] (2.4) The pH of the solution after mixing in step (2.3) is adjusted to 3.5 with a baking soda suspension, and the mixture is stirred at 5°C and pH 3.5 for 4 hours. The product obtained by the reaction is condensed with o-toluidine in a molar ratio of 1:1 to obtain dye Orange B.

[0068] The structural formula of the dye Orange B obtained is:

[0069] A method for preparing dye Yellow C, the specific steps are as follows:

[0070] (1) Preparation of intermediates:

[0071] (1.1) 5 g (16 mmol) of 3-amino-1,5-naphthalenedisulfonic acid (CAS 131-27-1) was added to 25 mL of chlorosulfonic acid at 0°C, the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 3-amino-1,5-naphthalenedisulfonyl chloride;

[0072] (1.2) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 3-amino-1,5-naphthalene disulfonyl chloride and 1 mmol of ethanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a diazo component;

[0073] (1.3) Add the diazo component to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11;

[0074] (1.4) Sodium carbonate is added to the diazonium salt solution to adjust the pH to 5, and m-methylaniline is added while the temperature is maintained at 10°C to cause a coupling reaction to produce an intermediate; wherein the molar ratio of the diazonium salt to m-methylaniline is 1:1.

[0075] (2) Synthesis of dyes, the specific steps are as follows:

[0076] (2.1) adding flake ice to water, stirring, adding an ice-grinding aid (the volume percentage composition of the ice-grinding aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-grinding 1,3,5-trifluoro-s-triazine for 5 minutes to obtain ice-grinded 1,3,5-trifluoro-s-triazine;

[0077] (2.2) adding the intermediate to water, adjusting the pH to 4 with sodium carbonate to dissolve the intermediate, and obtaining an intermediate solution;

[0078] (2.3) Cooling the intermediate solution to 10°C with ice, and then adding it to the 1,3,5-trifluoro-s-triazine ground with ice in step (2.1), maintaining the temperature at 0°C and pH = 3; wherein the molar ratio of the intermediate to 1,3,5-trifluoro-s-triazine is 1:1;

[0079] (2.4) The pH of the solution obtained in step (2.3) was adjusted to 3.5 with a baking soda suspension, and the mixture was stirred at 0°C and pH 3.5 for 4 hours to obtain Dye Yellow C.

[0080] The structural formula of the obtained dye yellow C is:

[0081] A method for preparing dye red D, the specific steps are as follows:

[0082] (1) Preparation of intermediates:

[0083] (1.1) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of o-aminobenzenesulfonyl chloride and 0.5 mmol of propanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine to catalyze the reaction to obtain a diazo component;

[0084] (1.2) Add the diazo component to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11;

[0085] (1.3) 5 g (16 mmol) of H acid (CAS 90-20-0) was added to 25 mL of chlorosulfonic acid at 0°C, the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 2-amino-4,7-dichlorosulfonylnaphthol;

[0086] (1.4) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 2-amino-4,7-dichlorosulfonylnaphthol and 1 mmol of propanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a coupling component;

[0087] (1.5) Sodium carbonate is added to the diazonium salt solution obtained in step (1.2) to adjust the pH to 5, and a coupling component is added while maintaining the temperature at 10° C. to cause a coupling reaction to obtain an intermediate; wherein the molar ratio of the diazonium salt to the coupling component is 1:1.

[0088] (2) Synthesis of dyes, the specific steps are as follows:

[0089] (2.1) adding flake ice to water, stirring, adding an ice-grinding aid (the volume percentage composition of the ice-grinding aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-grinding 2,4-dichloro-5-fluoro-6-methylpyrimidine (CAS954220-98-5) for 5 minutes to obtain ice-grinded 2,4-dichloro-5-fluoro-6-methylpyrimidine;

[0090] (2.2) adding the intermediate into water, adjusting the pH to 4 with sodium carbonate to dissolve the intermediate, and obtaining an intermediate solution;

[0091] (2.3) Cooling the intermediate solution to 10° C. with ice, and then adding it to the 2,4-dichloro-5-fluoro-6-methylpyrimidine ground with ice in step (2.1), maintaining the temperature at 0° C. and pH = 3; wherein the molar ratio of the intermediate to 2,4-dichloro-5-fluoro-6-methylpyrimidine is 1:1;

[0092] (2.4) The pH of the solution mixed in step (2.3) was adjusted to 3.5 with a baking soda suspension, and the mixture was stirred at 0°C and pH 3.5 for 4 hours to obtain dye red D.

[0093] The structural formula of the dye red D obtained is:

[0094] A method for preparing dye Red E, the specific steps are as follows:

[0095] (1) Preparation of intermediates:

[0096] (1.1) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of o-aminobenzenesulfonyl chloride and 0.5 mmol of propanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine to catalyze the reaction to obtain a diazo component;

[0097] (1.2) Add the diazo component to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11;

[0098] (1.3) 5 g (16 mmol) of H acid (CAS 90-20-0) was added to 25 mL of chlorosulfonic acid at 0°C. The mixture was warmed to room temperature within 30 min and stirred for 2 h. The reaction mixture was added to ice water to obtain 2-amino-4,7-dichlorosulfonylnaphthol;

[0099] (1.4) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 2-amino-4,7-dichlorosulfonylnaphthol and 1 mmol of propanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a coupling component;

[0100] (1.5) Sodium carbonate is added to the diazonium salt solution to adjust the pH to 5, and the coupling component is added while maintaining the temperature at 10°C to allow a coupling reaction to occur to obtain an intermediate; wherein the molar ratio of the diazonium salt to the coupling component is 1:1.

[0101] (2) Synthesis of dyes, the specific steps are as follows:

[0102] (2.1) adding flake ice to water, stirring, adding an ice-grinding aid (the volume percentage composition of the ice-grinding aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-grinding 2,4,5,6-tetrachloropyrimidine (CAS 1780-40-1) for 5 minutes to obtain ice-grinded 2,4,5,6-tetrachloropyrimidine;

[0103] (2.2) adding the intermediate into water, adjusting the pH to 4 with sodium carbonate to dissolve the intermediate, and obtaining an intermediate solution;

[0104] (2.3) Cooling the intermediate solution to 10° C. with ice, and then adding it to the 2,4,5,6-tetrachloropyrimidine ground with ice in step (2.1) to maintain the temperature at 0° C. and pH = 3; wherein the molar ratio of the intermediate to 2,4,5,6-tetrachloropyrimidine is 1:1;

[0105] (2.4) The pH of the solution mixed in step (2.3) was adjusted to 3.5 with a baking soda suspension, and the mixture was stirred at 0°C and pH 3.5 for 4 hours to obtain Dye Red E.

[0106] The structural formula of the dye Red E obtained is:

[0107] A method for preparing dye Red F, the specific steps are as follows:

[0108] (1) Preparation of intermediates:

[0109] (1.1) Add 5 g (22 mmol) of 1-naphthol-5-sulfonic acid (CAS 117-59-9) to 25 mL of chlorosulfonic acid at 0°C, warm the mixture to room temperature within 30 min, stir for 2 h, and add the reaction mixture into ice water to obtain 1-naphthol-5-sulfonyl chloride;

[0110] (1.2) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 1-naphthol-5-sulfonyl chloride and 0.5 mmol of tert-butanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a coupling component;

[0111] (1.3) Add 2-[(3-amino-4-methoxyphenyl)sulfonyl]ethanol to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11.

[0112] (2) Synthesis of dyes, the specific steps are as follows:

[0113] (2.1) adding sodium carbonate to the diazonium salt solution obtained in step (1.3) to adjust the pH to 5, adding the coupling component obtained in step (1.2) while maintaining the temperature at 10° C., and reacting for 2 h, then filtering, washing, and drying the precipitate; wherein the molar ratio of the diazonium salt to the coupling component is 1:1;

[0114] (2.2) Add the precipitate from step (2.1) and sodium acetate to acetic anhydride, and carry out acetylation reaction at 65° C. for 30 min. The molar ratio of the three is 1:1:1. After the reaction is completed, add the reaction solution to water, separate and dry to obtain dye red F.

[0115] The structural formula of the dye Red F obtained is:

[0116] A method for preparing dye Yellow G, the specific steps are as follows:

[0117] (1) Preparation of intermediates:

[0118] (1.1) 5 g (16 mmol) of 7-amino-1,3-naphthalene disulfonic acid (CAS 86-65-7) was added to 25 mL of chlorosulfonic acid at 0°C, the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 7-amino-1,3-naphthalene disulfonyl chloride;

[0119] (1.2) Add 2 mL of dichloromethane to a reaction vessel, add 0.5 mmol of 7-amino-1,3-naphthalene disulfonyl chloride and 1 mmol of trifluoroethanol together for esterification, and add 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a diazo component;

[0120] (1.3) Add the diazo component to a reaction vessel, add hydrochloric acid, cool to 0°C, add sodium nitrite and react in an ice bath at 0°C for 1.5 hours to obtain a diazonium salt solution; wherein the molar ratio of the diazo component, hydrochloric acid and sodium nitrite is 10:25:11;

[0121] (1.4) 2 mL of dichloromethane was added to a reaction vessel, and 0.5 mmol of m-acetamidoaniline formic acid and 0.5 mmol of tert-butyl alcohol were added together for esterification, and 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine was added for catalytic reaction to obtain a coupling component.

[0122] (2) Synthesis of dye: Sodium carbonate was added to the diazonium salt solution obtained in step (1.3) to adjust the pH to 5. The coupling component obtained in step (1.4) was added at a molar ratio of 1:1 while maintaining the temperature at 10°C. A coupling reaction occurred to obtain Dye Yellow G.

[0123] The structural formula of the obtained dye yellow G is:

[0124] A method for preparing dye red H, the specific steps are as follows:

[0125] (1) Preparation of intermediates:

[0126] The preparation method of intermediate A is as follows:

[0127] (a) adding aniline (Shanghai Yuanye Biotechnology Co., Ltd.) into a reaction vessel, adding hydrochloric acid, cooling to 0°C, adding sodium nitrite and reacting in an ice bath at 0°C for 1.5 hours to prepare a diazonium salt solution; wherein the molar ratio of aniline, hydrochloric acid and sodium nitrite is 10:25:11;

[0128] (b) adding 5 g (16 mmol) of H acid (CAS 90-20-0) to 25 mL of chlorosulfonic acid at 0° C., warming the mixture to room temperature within 30 min, stirring for 2 h, and adding the reaction mixture to ice water to obtain 2-amino-4,7-dichlorosulfonylnaphthol;

[0129] (c) adding 2 mL of dichloromethane to a reaction container, adding 0.5 mmol of 2-amino-4,7-dichlorosulfonylnaphthol and 1 mmol of 2,2-dimethylpropanol together for esterification, and adding 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine for catalytic reaction to obtain a coupling component;

[0130] (d) adding sodium carbonate to the diazonium salt solution obtained in step (a) to adjust the pH to 5, adding a coupling component while maintaining the temperature at 10° C. to cause a coupling reaction to obtain an intermediate A; wherein the molar ratio of the diazonium salt to the coupling component is 1:1.

[0131] The preparation method of intermediate B is as follows:

[0132] (I) 5 g (16 mmol) of 3-amino-1,5-naphthalenedisulfonic acid (CAS 131-27-1) was added to 25 mL of chlorosulfonic acid at 0° C., the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 3-amino-1,5-naphthalenedisulfonyl chloride;

[0133] (II) 2 ml of dichloromethane was added to a reaction vessel, and 0.5 mmol of 3-amino-1,5-naphthalene disulfonyl chloride and 1 mmol of 2,2-dimethylpropanol were added together for esterification, and 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine was added to catalyze the reaction to obtain an intermediate B.

[0134] (2) Synthesis of dyes, the specific steps are as follows:

[0135] (2.1) adding flake ice to water, stirring, adding an ice-grinding aid (the volume percentage composition of the ice-grinding aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-grinding 1,3,5-trichloro-s-triazine for 5 minutes to obtain ice-grinded 1,3,5-trichloro-s-triazine;

[0136] (2.2) Add intermediates A and B to water respectively, adjust the pH to 4 with sodium carbonate to dissolve intermediates A and B, and obtain intermediate A solution and intermediate B solution;

[0137] (2.3) Cooling the intermediate A solution and the intermediate B solution to 10°C with ice, and then adding them to the 1,3,5-trichloro-s-triazine ground with ice in step (2.1), maintaining the temperature at 0°C and pH = 3; wherein the molar ratio of intermediate A, intermediate B, and 1,3,5-trichloro-s-triazine is 1:1:1;

[0138] (2.4) The pH of the solution mixed in step (2.3) was adjusted to 3.5 with a baking soda suspension, and the mixture was stirred at 0°C and pH 3.5 for 4 hours to obtain dye red H.

[0139] The structural formula of the dye Red H obtained is:

[0140] A method for preparing dye blue I, the specific steps are as follows:

[0141] (1) Preparation of intermediates:

[0142] (1.1) 5 g (13 mmol) of 1-amino-4-bromoanthraquinone-2-sulfonic acid (CAS 116-81-4) was added to 25 mL of chlorosulfonic acid at 0°C; the mixture was warmed to room temperature within 30 min, stirred for 2 h, and the reaction mixture was added to ice water to obtain 1-amino-2-chlorosulfonyl-4-bromoanthraquinone;

[0143] (1.2) 2 mL of dichloromethane was added to a reaction vessel, and 0.5 mmol of 1-amino-2-chlorosulfonyl-4-bromoanthraquinone and 0.5 mmol of trifluoroethanol were added together for esterification, and 1 mL of a dichloromethane solution containing 0.6 mmol of triethylenediamine was added to catalyze the reaction to obtain an intermediate.

[0144] (2) Synthesis of dyes, the specific steps are as follows:

[0145] (2.1) adding flake ice to water, stirring, adding an ice-milling aid (the volume percentage of the ice-milling aid is 30% of dioxane, 30% of triethanolamine, 30% of chloroform, and 10% of acetic acid), and ice-milling the o-methoxy-para-ester for 5 minutes to obtain an ice-milled o-methoxy-para-ester;

[0146] (2.2) adding the intermediate into water, adjusting the pH to 4 with sodium carbonate to dissolve the intermediate, and obtaining an intermediate solution;

[0147] (2.3) Cooling the intermediate solution to 10° C. with ice, and then adding it to the o-methoxy-para-ester ground with ice in step (2.1), maintaining the temperature at 0° C. and pH at 3; wherein the molar ratio of the intermediate to the o-methoxy-para-ester is 1:1;

[0148] (2.4) adjusting the pH of the mixed solution in step (2.3) to 3.5 with a baking soda suspension, stirring at 0°C and pH 3.5 for 4 hours, and then filtering, washing, and drying the precipitate;

[0149] (2.5) Add the precipitate of step (2.4) and sodium acetate to acetic anhydride, and carry out acetylation reaction at 65° C. for 30 min. The molar ratio of the three is 1:1:1. After the reaction is completed, add the reaction solution to water, separate and dry to obtain dye blue I.

[0150] The structural formula of the obtained dye blue I is:

[0151] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0152] (1) Preparation of raw materials:

[0153] Cellulose fiber fabrics;

[0154] Alkaline solution: concentration 10 -3 mol / L, pH 8.593 sodium hydrogen phosphate solution;

[0155] Disperse reactive dye solution: Dye Blue A prepared in Example 1 was dissolved in isooctane to prepare a disperse reactive dye solution with a concentration of 0.5 g / L;

[0156] (2) placing the cellulose fiber fabric in an alkaline solution for swelling to obtain a wet fiber fabric with a liquid carrying rate of 40%;

[0157] (3) placing the wet fiber fabric in a disperse reactive dye solution at a bath ratio of 1:20, and dyeing at 45° C. for 1 hour to obtain a dyed fiber fabric; wherein the amount of dye used in the dyeing process is 1% omf.

[0158] The color absorption rate of the dyed fiber fabric is 97.50%, the color fixation rate is 93.20%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 5; 10 points are taken from the dyed fiber fabric to measure the LAB value, and the CIELAB color difference between the 10 points is 0.22.

[0159] Embodiment 11

[0160] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0161] (1) Preparation of raw materials:

[0162] Cellulose fiber fabrics;

[0163] Alkaline solution: concentration 10-6 mol / L, pH 8 sodium hydroxide solution;

[0164] Disperse reactive dye solution: Dye Orange B prepared in Example 2 was dissolved in liquid paraffin (Greagent brand of Shanghai Titan Technology Co., Ltd., CAS: 8012-95-1) to prepare a disperse reactive dye solution with a concentration of 1 g / L;

[0165] (2) placing the cellulose fiber fabric in an alkaline solution for swelling to obtain a wet fiber fabric with a liquid carrying rate of 55%;

[0166] (3) placing the wet fiber fabric in a disperse reactive dye solution at a bath ratio of 1:30, and dyeing at 50° C. for 1.5 hours to obtain a dyed fiber fabric; wherein the amount of dye used in the dyeing process is 3% omf.

[0167] The color absorption rate of the dyed fiber fabric is 96.30%, the color fixation rate is 92.80%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed fiber fabric to measure the LAB value, and the CIELAB color difference between the 10 points is 0.31.

[0168] Example 12

[0169] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0170] (1) Preparation of raw materials:

[0171] Cellulose fiber fabrics;

[0172] Alkaline solution: concentration 5×10 -4 mol / L, pH 7.726 sodium acetate solution;

[0173] Disperse reactive dye solution: Dye Yellow C prepared in Example 3 was dissolved in mineral oil (Adamas brand of Shanghai Titan Technology Co., Ltd., CAS: 8042-47-5) to prepare a disperse reactive dye solution with a concentration of 0.1 g / L;

[0174] (2) placing the cellulose fiber fabric in an alkaline solution for swelling to obtain a wet fiber fabric with a liquid carrying rate of 30%;

[0175] (3) placing the wet fiber fabric in a disperse reactive dye solution at a bath ratio of 1:10, and dyeing at 40° C. for 0.6 h to obtain a dyed fiber fabric; wherein the amount of dye used in the dyeing process is 0.1% omf.

[0176] The color absorption rate of the dyed fiber fabric is 98.50%, the color fixation rate is 94.20%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 5; 10 points are taken from the dyed fiber fabric to measure the LAB value, and the CIELAB color difference between the 10 points is 0.25.

[0177] Embodiment 13

[0178] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0179] (1) Preparation of raw materials:

[0180] Cellulose fiber fabrics;

[0181] Alkaline solution: concentration 2×10 -3 mol / L, pH 8.833 sodium bicarbonate solution;

[0182] Disperse reactive dye solution: Dye Red D prepared in Example 4 was dissolved in anisole to prepare a disperse reactive dye solution having a concentration of 0.33 g / L;

[0183] (2) placing the cellulose fiber fabric in an alkaline solution for swelling to obtain a wet fiber fabric with a liquid carrying rate of 35%;

[0184] (3) placing the wet fiber fabric in a dispersed reactive dye solution at a bath ratio of 1:15, and dyeing at 60° C. for 0.8 h to obtain a dyed fiber fabric; wherein the amount of dye used in the dyeing process is 0.5% omf.

[0185] The color absorption rate of the dyed fiber fabric is 98.90%, the color fixation rate is 93.60%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 5; 10 points are taken from the dyed fiber fabric to measure the LAB value, and the CIELAB color difference between the 10 points is 0.26.

[0186] Embodiment 14

[0187] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0188] (1) Preparation of raw materials:

[0189] Cellulose yarn;

[0190] Alkaline solution: concentration 10 -5 mol / L, pH 9 potassium hydroxide solution;

[0191] Disperse reactive dye solution: Dye Red E prepared in Example 5 was dissolved in dimethyl carbonate to prepare a disperse reactive dye solution with a concentration of 0.375 g / L;

[0192] (2) placing the cellulose yarn in an alkaline solution for swelling to obtain a wet yarn with a liquid content of 30%;

[0193] (3) placing the wet yarn in a disperse reactive dye solution at a bath ratio of 1:40, and dyeing at 75° C. for 1.5 hours to obtain a dyed yarn; wherein the amount of dye used in the dyeing process is 1.5% omf.

[0194] The color absorption rate of the dyed yarn is 96.70%, the color fixation rate is 93.40%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed yarn to measure the LAB value, and the CIELAB color difference between the 10 points is 0.24.

[0195] Embodiment 15

[0196] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0197] (1) Preparation of raw materials:

[0198] Cellulose yarn;

[0199] Alkaline solution: concentration 10 -4 mol / L, pH 9.5 sodium silicate solution;

[0200] Disperse reactive dye solution: Dye Red F prepared in Example 6 was dissolved in decamethylcyclopentasiloxane (Adamas brand of Shanghai Titan Technology Co., Ltd., CAS: 541-02-6) to prepare a disperse reactive dye solution with a concentration of 0.33 g / L;

[0201] (2) placing the cellulose yarn in an alkaline solution for swelling to obtain a wet yarn with a liquid content of 50%;

[0202] (3) placing the wet yarn in a disperse reactive dye solution at a bath ratio of 1:60, and dyeing at 85° C. for 1.2 hours to obtain a dyed yarn; wherein the dye dosage in the dyeing process is 2% omf.

[0203] The color absorption rate of the dyed yarn is 97.30%, the color fixation rate is 92.90%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 4, the color change fastness is level 4-5, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed yarn to measure the LAB value, and the CIELAB color difference between the 10 points is 0.37.

[0204] Example 16

[0205] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0206] (1) Preparation of raw materials:

[0207] Cellulose yarn;

[0208] Alkaline solution: concentration 10 -4 mol / L, pH 10.991 sodium phosphate solution;

[0209] Disperse reactive dye solution: Dye Yellow G prepared in Example 7 was dissolved in octamethylcyclotetrasiloxane (Adamas brand of Shanghai Titan Technology Co., Ltd., CAS: 556-67-2) to prepare a disperse reactive dye solution with a concentration of 1 g / L;

[0210] (2) placing the cellulose yarn in an alkaline solution for swelling to obtain a wet yarn with a liquid carrying rate of 80%;

[0211] (3) placing the wet yarn in a disperse reactive dye solution at a bath ratio of 1:80, and dyeing at 100° C. for 2 hours to obtain a dyed yarn; wherein the dye dosage in the dyeing process is 8% omf.

[0212] The color absorption rate of the dyed yarn is 96.20%, the color fixation rate is 91.80%, the dry rubbing fastness is level 4-5, the wet rubbing fastness is level 3-4, the color change fastness is level 4, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed yarn to measure the LAB value, and the CIELAB color difference between the 10 points is 0.45.

[0213] Embodiment 17

[0214] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0215] (1) Preparation of raw materials:

[0216] Cellulose yarn;

[0217] Alkaline solution: concentration 10 -3 mol / L, pH 10.534 sodium carbonate solution;

[0218] Disperse reactive dye solution: The dye Red H prepared in Example 8 was dissolved in edible oil (Luhua Fragrant Soybean Oil, Shandong Luhua Group Co., Ltd.) to prepare a disperse reactive dye solution with a concentration of 0.615 g / L;

[0219] (2) placing the cellulose yarn in an alkaline solution for swelling to obtain a wet yarn with a liquid content of 60%;

[0220] (3) placing the wet yarn in a disperse reactive dye solution at a bath ratio of 1:65, and dyeing at 80° C. for 1.6 hours to obtain a dyed yarn; wherein the dye dosage in the dyeing process is 4% omf.

[0221] The color absorption rate of the dyed yarn is 95.80%, the color fixation rate is 92.30%, the dry rubbing fastness is level 5, the wet rubbing fastness is level 3-4, the color change fastness is level 4-5, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed yarn to measure the LAB value, and the CIELAB color difference between the 10 points is 0.39.

[0222] Embodiment 18

[0223] A non-aqueous medium dyeing process of disperse reactive dyes with convertible affinity, the specific steps are as follows:

[0224] (1) Preparation of raw materials:

[0225] Cellulose yarn;

[0226] Alkaline solution: concentration 10 -3 mol / L, pH 9.099 sodium hydrogen phosphate solution and concentration 10 -3 mol / L, a mixture of sodium phosphate solutions with a pH of 10.991; wherein the volume ratio of the sodium hydrogen phosphate solution to the sodium phosphate solution is 1:1;

[0227] Disperse reactive dye solution: Dye Blue I prepared in Example 9 was dissolved in supercritical CO 2 fluid, to prepare a disperse reactive dye solution with a concentration of 0.8 g / L;

[0228] (2) placing the cellulose yarn in an alkaline solution for swelling to obtain a wet yarn with a liquid content of 70%;

[0229] (3) placing the wet yarn in a disperse reactive dye solution at a bath ratio of 1:75, and dyeing the yarn at 90° C. for 1.8 hours to obtain a dyed yarn; wherein the dye dosage in the dyeing process is 6% omf.

[0230] The color absorption rate of the dyed yarn is 95.40%, the color fixation rate is 91.60%, the dry rubbing fastness is level 4-5, the wet rubbing fastness is level 3-4, the color change fastness is level 4, and the cotton staining fastness is level 4-5; 10 points are taken from the dyed yarn to measure the LAB value, and the CIELAB color difference between the 10 points is 0.41.

Claims

1. A non-aqueous dyeing process for disperse reactive dyes with variable affinity, Features: placing the wet fabric or yarn in a disperse reactive dye solution for dyeing to obtain a dyed fabric or yarn; The wet fabric or yarn is obtained by swelling the cellulose fiber fabric or yarn in an alkaline solution with a pH of 7.5 to 11; The disperse reactive dye solution is a solution obtained by dissolving a disperse reactive dye with convertible affinity in a weakly polar or non-polar solvent with a relative dielectric constant of less than 5; Affinity-convertible disperse reactive dyes are disperse reactive dyes that contain affinity-convertible groups and reactive groups in their molecular structures. Under alkaline conditions of pH 7.5 to 11, the reactivity of the affinity-convertible groups with water is greater than the reactivity of the reactive groups with cellulose. The affinity-convertible group is a fluorosulfonyl group or a sulfonate group.

2. The process for dyeing disperse reactive dyes with convertible affinity according to claim 1, It is characterized in that The liquid carrying rate of the wet fabric or yarn is 30 to 80%.

3. The process for dyeing disperse reactive dyes with convertible affinity according to claim 1, It is characterized in that The active group is a vinylsulfone type active group, an s-triazine type active group, a pyrimidine type active group or a carbamate type active group.

4. The process for dyeing disperse reactive dyes in non-aqueous medium with convertible affinity according to claim 1, It is characterized in that Weakly polar or non-polar solvents with a relative dielectric constant of less than 5 are isooctane, liquid paraffin, mineral oil, anisole, dimethyl carbonate, silicones, edible oil or supercritical CO 2 fluid.

5. The process for dyeing disperse reactive dyes with convertible affinity according to claim 1, It is characterized in that The dyeing temperature is 40-100°C and the dyeing time is 0.5-2h.

6. The process for dyeing disperse reactive dyes in non-aqueous medium with convertible affinity according to claim 1, It is characterized in that The bath ratio during dyeing is 1:10-100, and the amount of dye used in the dyeing process is 0.1-10% omf.

7. The process for dyeing disperse reactive dyes in non-aqueous medium with convertible affinity according to claim 1, It is characterized in that The alkaline solution is one or more of a sodium carbonate solution, a sodium bicarbonate solution, a sodium hydroxide solution, a potassium hydroxide solution, a sodium silicate solution, a sodium phosphate solution, a sodium hydrogen phosphate solution and a sodium acetate solution.

8. The process for dyeing disperse reactive dyes in non-aqueous medium with convertible affinity according to claim 7, It is characterized in that The concentration of alkaline solution is 10 -7 ~10 -2 mol / L.

9. The process for dyeing disperse reactive dyes in non-aqueous medium with convertible affinity according to claim 1, It is characterized in that The concentration of disperse reactive dye solution is 0.01-5 g / L.

10. A process for dyeing disperse reactive dyes in non-aqueous medium with variable affinity according to any one of claims 1 to 9, It is characterized in that The dyed fabric or yarn has a color absorption rate greater than 95%, a color fixation rate greater than 90%, a dry rubbing fastness greater than grade 4, a wet rubbing fastness greater than grade 3-4, a color change fastness greater than grade 4, and a cotton staining fastness greater than grade 4-5. Take 10 points from the dyed fabric or yarn to measure the LAB value, and the CIELAB color difference between the 10 points is <0.5.