A short-process polyester color fixing process

Abstract

The invention discloses a short-process polyester color fixing process, which includes: dyeing → washing → padding with color fixing working solution → heat treatment → heat setting. The invention adds a polymer dyeing promoter with pH responsiveness in the dyeing stage, so as to improve the dyeing rate of disperse dyes on the one hand, and adjust the pH to alkaline after dyeing to hydrolyze it on the other hand, and the hydrolyzate is used as a color fixing auxiliary agent to fix the color with the color fixing working solution in the heat treatment section; the obtained polyester fabric has a high color fixing rate and color fastness, and the process flow eliminates the complicated reduction cleaning and multi-step washing sections.

Description

Technical Field

[0001] The invention belongs to the field of polyester printing and dyeing, and specifically relates to a short-process polyester color fixing process. Background Art

[0002] Polyester fiber is a hydrophobic synthetic fiber. The molecular structure of polyester lacks active groups that can bind to dyes like cellulose or protein fibers. In addition, the polyester molecules are arranged relatively tightly, and there are only small gaps in the fiber, so disperse dyes are difficult to penetrate into the fiber. Therefore, it is generally necessary to add a dyeing accelerator to plasticize the polyester fiber to increase the diffusion of disperse dyes inside the fiber. On the other hand, since disperse dyes are bound to polyester fibers through non-covalent bonds, reduction cleaning is required after dyeing in order to destroy and wash out the dyes that have not entered the fiber and improve color fastness. In addition, a fixing agent needs to be added for finishing to prevent the disperse dyes inside the fiber from migrating to the fiber surface under heat during the subsequent baking process.

[0003] In the prior art, a mixed formula of insurance powder and caustic soda is usually used to reduce and clean the dyed polyester, and then it needs to be repeatedly washed with water until it is neutral. Although this method is simple to operate, economical and has good color fixing effect, it has the following problems: 1. Insurance powder will spontaneously combust when it comes into contact with water, which has a very high fire hazard; 2. Insurance powder has poor stability and is easily decomposed in a hot and humid environment, resulting in a decrease in reducing power and affecting the effect; 3. Insurance powder has poor heat resistance and stability, and it disperses quickly in water above 60°C, and its effective utilization rate is low; 4. It has high operating requirements, and uneven color fixing (color flower) is prone to occur if the material is not thoroughly oxidized; 5. The residual liquid after color fixing is reducing, and the amount of washing water used is large, which increases the burden of sewage treatment.

[0004] In view of this, the present invention is proposed. Summary of the invention

[0005] The invention provides a short-process polyester color fixing process, aiming to solve the problems of long process flow and large water consumption in the prior art of polyester color fixing.

[0006] The present invention is achieved through the following technical solutions:

[0007] A short-process polyester color fixing process comprises the following steps:

[0008] (1) dyeing: immersing the polyester fabric in a dye bath for dyeing; after dyeing, adding alkali to adjust the pH value to above 10 for hydrolysis reaction, and draining the water after dyeing; the dye bath includes disperse dyes and polymer leveling agents;

[0009] (2) washing: washing the dyed polyester obtained in step (1);

[0010] (3) dipping in a color fixing working solution, wherein the color fixing working solution comprises an epoxy compound and deionized water;

[0011] (4) Heat treatment;

[0012] (5) Heat setting;

[0013] The polymer leveling agent has the following molecular structure:

[0014]

[0015] In the formula, R1 and R2 are independently selected from H or CH3; R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, CH2CH(CH3)OH; R4 is selected from a straight-chain alkyl group having 7 to 11 carbon atoms; the ratio of x to y is 1:2 to 4, and the value of x is 3 to 15.

[0016] In some embodiments of the present invention, the dyeing temperature in step (1) is 100-140° C., the dyeing time is 20-40 min, and the bath ratio is (1:10-20).

[0017] In some embodiments of the present invention, after dyeing, alkali is added to adjust the pH value of the dye bath to 10-12; the alkali is selected from at least one of sodium carbonate, sodium hydroxide, potassium hydroxide and ammonia water.

[0018] In some embodiments of the present invention, the temperature of the hydrolysis reaction is 60-80° C., and the time is 15-30 min.

[0019] In some embodiments of the present invention, the dye bath formula includes: 1-2% (owf) disperse dye, 1-2 g / L polymer leveling agent, and 0.5-1.5 g / L glacial acetic acid.

[0020] Furthermore, the preparation steps of the polymer leveling agent are as follows:

[0021] S1: mixing phenylboronic acid monomer and hydrophilic monomer in a first solvent, adding an initiator to carry out polymerization reaction, and obtaining a copolymer;

[0022] S2: The copolymer and the diethanolamine monomer are mixed in a second solvent and stirred under alkaline conditions to obtain a polymer leveling agent.

[0023] The copolymer has the structure of formula III:

[0024]

[0025] In the formula, R1 and R2 are independently selected from H or CH3; R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, CH2CH(CH3)OH; the ratio of x to y is 1:2-4, and the value of x is 3-15.

[0026] In some embodiments of the present invention, step S1 meets at least one of the following features 1 to 6:

[0027] Feature 1: The first solvent is at least one of N,N-dimethylformamide DMF, dimethyl sulfoxide DMSO, and N,N-dimethylacetamide DMAc;

[0028] Feature 2: The phenylboronic acid monomer is 3-acrylamide phenylboronic acid or 3-methacrylamide phenylboronic acid;

[0029] Feature 3: The hydrophilic monomer is selected from at least one of methacrylic acid, acrylic acid, hydroxyethyl methacrylate, hydroxyethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, and hydroxypropyl methacrylate;

[0030] Feature 4: The initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptanenitrile, dimethyl azobisisobutyrate, and 4,4-azo(4-cyanovaleric acid);

[0031] Feature 5: The polymerization reaction is carried out in an inert atmosphere, the reaction temperature is 80-120°C, and the reaction time is 2-6 hours;

[0032] Feature 6: The molar ratio of the phenylboronic acid monomer and the hydrophilic monomer is 1:1-5, and the amount of the initiator added is 1%-3% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

[0033] In some embodiments of the present invention, step S2 meets at least one of the following features 1 to 6:

[0034] Feature 1: The diethanolamine monomer is selected from at least one of N,N-bis(2-hydroxyethyl)octanamide, N,N-bis(2-hydroxyethyl)nonanamide, N,N-bis(2-hydroxyethyl)decanamide, N,N-bis(2-hydroxyethyl)undecanamide and N,N-bis(2-hydroxyethyl)dodecanamide;

[0035] Feature 2: The second solvent is at least one of methanol, ethanol, isopropanol, and ethylene glycol;

[0036] Characteristic 3: Alkaline conditions refer to adding acid or base to adjust the reaction pH to 9 ± 0.5;

[0037] Feature 4: Stirring reaction refers to stirring reaction at room temperature for 30 minutes.

[0038] Characteristic 5: The ratio of the molar amount of phenylboronic acid groups in the copolymer to the molar amount of diethanolamine monomer is 1:1.05-1.2;

[0039] Feature 6: The feeding ratio of the total mass of the copolymer and the diethanolamine monomer to the second solvent is 1g:200-400mL.

[0040] The polymer leveling agent provided by the present invention will be hydrolyzed when the pH is higher than 10, that is, when the pH is higher than 10, the polymer leveling agent having formula I can be hydrolyzed to obtain a compound of formula II,

[0041]

[0042] In the formula, R4 is selected from a straight-chain alkyl group having 7 to 11 carbon atoms.

[0043] The phenylboronic acid group in the copolymer main chain of the polymer leveling agent provided by the present invention is combined with the diethanolamine group in the side chain through a boron-nitrogen coordination reaction. Since the polymer leveling agent contains groups similar to those compatible with polyester, such as amide, ester, phenyl, etc., it can enter the polyester molecular chain under dye bath conditions to plasticize it.

[0044] After dyeing, alkali is added to adjust the pH of the dye bath to above 10. Under this condition, the polymer leveling agent undergoes a hydrolysis reaction, and the main chain and side chain of the copolymer are dissociated. Since the main chain of the copolymer is hydrophilic and its solubility is further enhanced under alkaline hydrolysis conditions, it is dissolved from the inside of the fiber and enters the liquid phase. The side chain diethanolamine monomer after hydrolysis is highly hydrophobic and adheres to the fiber surface, and can be used as one of the subsequent color fixing components.

[0045] In some embodiments of the present invention, the water washing temperature in step (2) is room temperature, the water washing time is 10 to 20 minutes, and the bath ratio is (1:10 to 20).

[0046] In some embodiments of the present invention, the formula of the color fixing working solution in step (3) includes: 40 to 50 parts of epoxy compounds, 4 to 10 parts of cationic compounds, 0 to 20 parts of polyols, and 10 to 30 parts of deionized water.

[0047] In some embodiments of the present invention, the epoxy compound is selected from at least one of oxychloropropane, glycidol, pentaerythritol glycidyl ether, glycidyl ether, and polyethylene glycol diglycidyl ether.

[0048] In some embodiments of the present invention, the cationic compound is selected from at least one of 3-chloro-2-hydroxypropyltrimethylammonium chloride and 2,3-epoxypropyltrimethylammonium chloride.

[0049] In some embodiments of the present invention, the polyol is selected from at least one of polyether polyol, triisopropanolamine, triethanolamine, and pentaerythritol.

[0050] The diethanolamine monomer obtained by hydrolyzing the polymer dyeing accelerator provided by the present invention adheres to the surface of the polyester and reacts with the epoxy compound in the color fixing auxiliary agent under heating conditions to form a polymer film on the surface of the polyester. In order to further improve the film-forming property and the softness of the fabric, a long-chain polyol can be added as an auxiliary.

[0051] The cationic compound is added to the color fixing working solution of the present invention to improve the hydrophilicity and skin affinity of the polyester fabric, and at the same time plays an antistatic role, thereby improving the skin affinity and wearability of the fabric to a certain extent.

[0052] In some embodiments of the present invention, the dipping and rolling in step (3) is one dipping and one rolling or two dipping and two rolling.

[0053] In some embodiments of the present invention, the padding liquid ratio in step (3) is 60% to 80%.

[0054] In some embodiments of the present invention, the heat treatment in step (4) refers to heating to 80-100° C. at a rate of 1-2° C. / min for 20-30 min.

[0055] In some embodiments of the present invention, the temperature of the heat setting in step (5) is 180-220°C.

[0056] The present invention has the following advantages and beneficial effects:

[0057] The invention provides a short-process polyester color fixing process, which adopts a self-made polymer dyeing accelerator to be added to the dye bath. The polymer dyeing accelerator has the characteristic of pH responsiveness, so that it acts as a switch, plasticizes the polyester in the acidic dye bath and plays a dyeing accelerator role; decomposes and precipitates in the alkaline bath, so that the plasticity of the polyester decreases, and the migration and precipitation of dye molecules during post-treatment are inhibited. In addition, the diethanolamine monomer obtained by the decomposition of the polymer dyeing accelerator is adsorbed on the surface of the polyester fiber due to its hydrophobicity, and reacts with the epoxy compound in the color fixing stage, thereby forming a polymer film on the fiber surface. The polymer film fixes the floating color to achieve the effect of non-reduction cleaning and color fixing, saving the process and reducing water consumption. BRIEF DESCRIPTION OF THE DRAWINGS

[0058] Figure 1 The following are the H-NMR spectra of the copolymer and polymer dyeing accelerator prepared in Example 1.

[0059] Figure 2 The hydrogen nuclear magnetic spectra of the copolymer of Example 1 and the polymer dyeing accelerator prepared in Example 1 under weakly acidic conditions (pH=4.5) and strongly alkaline conditions (pH=10).

[0060] Figure 3 This is the H-NMR spectrum of the liquid obtained by immersing the dyed and cold-washed fabric in Example 1 in DMSO at room temperature. DETAILED DESCRIPTION

[0061] The present invention is further described in detail below in conjunction with specific examples, but the examples do not limit the present invention in any form. Unless otherwise specified, the reagents, methods and equipment used in the present invention are conventional reagents, methods and equipment in the art.

[0062] The raw materials used in the specific implementation are described as follows: dyes were purchased from Zhejiang Longsheng Group Co., Ltd.; polyester (150D×150D) was purchased from Suzhou Fantesi Textile Co., Ltd.; polyether polyol (hydroxyl value 36-39 mgKOH / g, viscosity 25°C 500-600 mPa·s) was purchased from Shandong Dongda Chemical Group; polyethylene glycol glycidyl ether 205 (epoxy value 0.35) was purchased from Guangzhou Ruishi Biotechnology Co., Ltd.

[0063] The embodiment of the present invention provides a short-process polyester color fixing process, which adds a functional polymer dyeing accelerator in the dyeing stage and adjusts the conditions to make it play the role of dyeing promotion and color fixing at the same time, thereby reducing the color fixing process flow and eliminating reduction cleaning and multi-step water washing.

[0064] The embodiment of the present invention provides a short-process polyester color fixing process, comprising the following steps:

[0065] (1) Dyeing: The polyester fabric is immersed in a dye bath for dyeing; after the dyeing is completed, alkali is added to adjust the pH value to above 10 for hydrolysis reaction, and then the water is drained after the dyeing is completed.

[0066] (2) washing: washing the dyed polyester obtained in step (1);

[0067] (3) Padding and fixing working solution;

[0068] (4) Heat treatment;

[0069] (5) Heat setting;

[0070] The parameters in the process are described as follows:

[0071] In some embodiments, the dye bath formula is as follows: disperse dye 1-2% (owf), polymer leveling agent 1-2 g / L, glacial acetic acid 0.5-1.5 g / L.

[0072] Specifically, the disperse dye can be an azo disperse dye, anthraquinone disperse dye, heterocyclic disperse dye, etc. The amount of the disperse dye can be 1% (owf), 1.5% (oWf), 2% (owf), etc., or any value among the above adjacent values.

[0073] The polymer leveling agent has the following molecular structure:

[0074]

[0075] In the formula, R1 and R2 are independently selected from H or CH3; R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, CH2CH(CH3)OH; R4 is selected from a straight-chain alkyl group having 7 to 11 carbon atoms; the ratio of x to y is 1:2 to 4, and the value of x is 3 to 15.

[0076] The polymer dyeing accelerator having the molecular structure of Formula 1 is pH responsive and can undergo a hydrolysis reaction when the pH is higher than 10. The hydrolysis product has the structures of Formula II and Formula IV:

[0077]

[0078] In the formula, R4 is selected from a straight-chain alkyl group having 7 to 11 carbon atoms.

[0079]

[0080] In the formula,

[0081] R l and R2 is independently selected from H or CH3;

[0082] R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, and CH2CH(CH3)OH;

[0083] The ratio of x to y is 1:2-4, specifically, 1:2, 1:3, 1:4, etc.; the value of x is 3-15, specifically, 3, 5, 7, 10, 12, 15, etc., or any value among the above adjacent values. The present invention can demonstrate the product structure of the polymer dyeing accelerator by gel chromatography, nuclear magnetic resonance spectroscopy, mass spectrometry, etc.

[0084] The polymer leveling agent provided by the present invention has suitable hydrophilicity and hydrophobicity, so that it can be effectively dispersed in the dye bath and can migrate to the interior of the polyester after being put into the polyester cloth, so as to play a plasticizing and swelling effect on the polyester, so that the swelling rate of the fiber is increased and the glass transition temperature is reduced, which is beneficial for the disperse dye to diffuse inside the fiber to complete the dyeing. The plasticizing and swelling effect on the polyester is due to some groups and fragments with similar structures to the polyester, such as benzene ring, ester group, amide group, alkyl group, etc.

[0085] The compound of formula IV obtained by hydrolysis of the polymer dyeing accelerator under alkaline conditions has good water solubility and migrates from the interior of the fiber to the water phase. The compound of formula II has a similar structure to that of a surfactant, i.e., one end is hydrophilic and the other end is lipophilic, and also migrates from the interior of the fiber to the solid-liquid interface composed of the fiber and the water phase. Due to the migration and precipitation of the polymer dyeing accelerator, the plasticizing effect on the polyester disappears, and the activity of the polyester chain segment decreases, thereby inhibiting the precipitation of the disperse dye that has diffused into the interior and improving the color fixation rate. The compound of formula II, i.e., diethanolamine monomer, which remains at the solid-liquid interface, can be used as an auxiliary agent in subsequent color fixation finishing.

[0086] Specifically, the concentration of the polymer leveling agent in the dye bath can be 1 g / L, 1.5 g / L, 2 g / L, etc., or any value in the adjacent ranges above. The concentration of the polymer leveling agent has an influence on the fixation rate, and can be selected according to the type of disperse dye and the specification of the polyester fabric.

[0087] Specifically, the concentration of glacial acetic acid in the dye bath can be 0.5 g / L, 1 g / L, 1.5 g / L, etc., or any value among the above adjacent values. The concentration of glacial acetic acid has an effect on the pH of the dye bath, so that the pH of the dye bath is maintained at 4.5 to 7. Under this pH condition, disperse dyes have good stability and activity.

[0088] In some embodiments, the dyeing temperature is 100-140° C., the time is 20-40 min, and the bath ratio is (1:10-20). Different temperatures, times, and bath ratios are selected according to different disperse dyes or dye bath components so that the fabric has a good dyeing effect.

[0089] Specifically, the dyeing temperature can be 100°C, 110°C, 120°C, 130°C, 140°C, etc., the dyeing time can be 20min, 30min, 40min, etc., the bath ratio can be (1:10), (1:15), (1:20), etc., or any value among the above adjacent values.

[0090] In some embodiments of the present invention, after dyeing, alkali is added to adjust the pH value of the dye bath to 10-12; specifically, the pH value can be 10, 11, 12, etc., or any value among the adjacent values ​​above.

[0091] Specifically, the alkali is selected from at least one of sodium carbonate, sodium hydroxide, potassium hydroxide and ammonia water.

[0092] In some embodiments of the present invention, the temperature of the hydrolysis reaction is 60-80°C, and the time is 15-30 min. Specifically, the temperature of the hydrolysis reaction can be 60°C, 70°C, 80°C, etc., and the hydrolysis time can be 10 min, 20 min, 30 min, etc., or any value among the above adjacent values.

[0093] The steps for preparing the polymer dyeing accelerator provided by the present invention are as follows:

[0094] S1: mixing phenylboronic acid monomer and hydrophilic monomer in a first solvent, adding an initiator to carry out polymerization reaction, and obtaining a copolymer;

[0095] S2: The copolymer and the diethanolamine monomer are mixed in a second solvent and stirred under alkaline conditions to obtain a polymer leveling agent.

[0096] The copolymer has the structure of formula III:

[0097]

[0098] In the formula, R l and R2 is independently selected from H or CH3;

[0099] R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, and CH2CH(CH3)OH;

[0100] The ratio of x to y is 1:2-4, specifically, 1:2, 1:3, 1:4, etc.; the value of x is 3-15, specifically, 3, 5, 7, 10, 12, 15, etc., or any value among the above adjacent values. The present invention can demonstrate the product structure of the polymer dyeing accelerator by gel chromatography, nuclear magnetic resonance spectroscopy, mass spectrometry, etc.

[0101] In some embodiments of the present invention, the first solvent is at least one of N,N-dimethylformamide DMF, dimethyl sulfoxide DMSO, and N,N-dimethylacetamide DMAc;

[0102] In some embodiments of the present invention, the phenylboronic acid monomer is 3-acrylamide phenylboronic acid or 3-methacrylamide phenylboronic acid;

[0103] In some embodiments of the present invention, the hydrophilic monomer is selected from at least one of methacrylic acid, acrylic acid, hydroxyethyl methacrylate, hydroxyethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, and hydroxypropyl methacrylate;

[0104] In some embodiments of the present invention, the initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptanenitrile, dimethyl azobisisobutyrate, and 4,4-azo(4-cyanovaleric acid);

[0105] In some embodiments of the present invention, the polymerization reaction is carried out in an inert atmosphere, the reaction temperature is 80 to 120° C., and the reaction time is 2 to 6 hours;

[0106] In some embodiments of the present invention, the molar ratio of phenylboronic acid monomer and hydrophilic monomer is 1:(1-5), specifically, it can be 1:1, 1:2, 1:3, 1:4, 1:5, etc., or any value among the above adjacent values; the amount of initiator added is 1% to 3% of the total mass of phenylboronic acid monomer and hydrophilic monomer, specifically, it can be 1%, 2%, 3%, etc., or any value among the above adjacent values.

[0107] In some embodiments of the present invention, the diethanolamine monomer is selected from at least one of N,N-bis(2-hydroxyethyl)octanamide, N,N-bis(2-hydroxyethyl)nonanamide, N,N-bis(2-hydroxyethyl)decanamide, N,N-bis(2-hydroxyethyl)undecanamide, and N,N-bis(2-hydroxyethyl)dodecanamide;

[0108] In some embodiments of the present invention, the second solvent is at least one of methanol, ethanol, isopropanol, and ethylene glycol;

[0109] In some embodiments of the present invention, alkaline conditions refer to adding acid or base to adjust the reaction pH to 9±0.5;

[0110] In some embodiments of the present invention, the stirring reaction refers to stirring the reaction at room temperature for 30 minutes;

[0111] In some embodiments of the present invention, the ratio of the molar amount of phenylboronic acid groups in the copolymer to the molar amount of diethanolamine monomer is 1:1.05 to 1.2, specifically, it can be 1:1.05, 1:1.1, 1:1.2, etc., or any value among the adjacent values ​​above;

[0112] In some embodiments of the present invention, the total mass of the copolymer and diethanolamine monomer to the second solvent is 1g:200-400mL, specifically, it can be 1:200mL, 1:300mL, 1:400mL, etc., or any value among the above adjacent values.

[0113] In some embodiments of the present invention, the washing temperature in step (2) is room temperature, the washing time is 10 to 20 minutes, and the bath ratio is (1:10 to 20). The purpose of washing is to make the acidity and alkalinity of the fabric neutral to low alkalinity, and to wash away the attached metal salts such as sodium acetate, ammonium acetate, etc., and the hydrolysis products of the polymer dyeing accelerator.

[0114] In some embodiments of the present invention, the formula of the color fixing working solution in step (3) includes: 40-50 parts of epoxy compound, 4-10 parts of cationic compound, 0-20 parts of polyol, and 10-30 parts of deionized water. By adjusting the types and addition amounts of epoxy compound, cationic compound, and polyol, the film-forming property of the working solution can be regulated, thereby affecting the color fixing rate, the touch, hydrophilicity, and wearing performance of the fabric.

[0115] In some embodiments of the present invention, the epoxy compound is selected from at least one of oxychloropropane, glycidol, pentaerythritol glycidyl ether, glycidyl ether, and polyethylene glycol diglycidyl ether. The epoxy compound can undergo a ring-opening reaction with a hydroxyl group under heating conditions. Since the epoxy compound and the hydroxyl compound (the hydroxyl compound of the present invention is the hydrolysis product of the polymer dyeing accelerator, diethanolamine, and polyol) are both multifunctional, a three-dimensional cross-linked network membrane structure can be obtained through the ring-opening reaction to cover the fiber surface, thereby achieving the purpose of color fixation.

[0116] In some embodiments of the present invention, the cationic compound is selected from at least one of 3-chloro-2-hydroxypropyltrimethylammonium chloride and 2,3-epoxypropyltrimethylammonium chloride.

[0117] In some embodiments of the present invention, the polyol is selected from at least one of polyether polyol, triisopropanolamine, triethanolamine, and pentaerythritol. The role of the polyol is to supplement and dilute diethanolamine. On the one hand, the atomic distance between the two alcohol hydroxyl groups of diethanolamine is small, which will make the cross-linking density of the system too large. Adding long-chain polyols such as polyether polyols can reduce the cross-linking density and play a diluting role, so that the system has better film-forming properties; on the other hand, since the diethanolamine monomer has a long-chain hydrophobic alkyl group, its hydrophobic effect is strong, and the addition of hydrophilic polyol monomers can adjust the hydrophilicity and skin-friendliness of the resulting polyester fabric, but the addition of polyols is not necessary. In some embodiments of the present invention, adding polymer-type epoxy compounds can also play a similar role, and the performance is better.

[0118] In some embodiments of the present invention, the dipping and rolling in step (3) is one dipping and one rolling or two dipping and two rolling.

[0119] In some embodiments of the present invention, the padding liquid ratio in step (3) is 60% to 80%, specifically, it can be 60, 70, 80, etc., or any value among the adjacent values ​​above.

[0120] In some embodiments of the present invention, the heat treatment in step (4) refers to heating the temperature to 80-100° C. for 20-30 min at a heating rate of 1-2° C. / min. Specifically, the heating rate is controlled so that it is in a relatively slow heating process, which is conducive to the ring-opening reaction of the epoxy compound and the hydroxyl-containing compound, so that the fluidity of each component before film formation is better, and the obtained film has better uniformity, which is conducive to improving color fastness, fabric touch and wearing performance.

[0121] In some embodiments of the present invention, the temperature of the heat setting in step (5) is 180-220°C.

[0122] Example 1

[0123] A short-process polyester color fixing process comprises the following steps:

[0124] (1) Dyeing: The polyester fabric is immersed in a dye bath for dyeing at a bath ratio of 1:10, a temperature of 120°C, and a time of 30 minutes. After dyeing, wait for the dye bath to cool to 70°C, add alkali to adjust the pH value to 10, and continue to keep warm for 20 minutes to allow the polymer leveling agent to be fully hydrolyzed, and then drain the water.

[0125] The dye bath formula is as follows: C, I. Disperse red 1772% (owf), polymer leveling agent 1.5 g / L, glacial acetic acid 1 g / L.

[0126] The preparation method of the polymer leveling agent is as follows:

[0127] S1: Mix 3v acrylamidophenylboronic acid and hydrophilic monomer in DMF, add azobisisobutyronitrile (AIBN) under nitrogen protection and react at 100°C for 4h, pour the obtained reaction solution into twice the volume of water for precipitation, filter the obtained precipitate, wash it with deionized water for 3 times, and dry it at 80°C to constant weight to obtain a copolymer;

[0128] The hydrophilic monomer is hydroxyethyl methacrylate.

[0129] The molar ratio of the phenylboronic acid monomer to the total molar ratio of the hydrophilic monomer is 1:4; the added amount of the initiator is 2% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

[0130] S2: After the copolymer and N, N-bis(2-hydroxyethyl)decylamide are mixed in ethanol, NaOH is added to adjust the pH of the reaction solution to 9, and then the reaction is stirred at room temperature for 30 minutes. The obtained reaction solution is poured into twice the volume of water for precipitation, and the precipitate is filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a polymer leveling agent.

[0131] The molar ratio of the phenylboronic acid group in the copolymer to the molar ratio of N, N-bis(2-hydroxyethyl)decylamide is 1:1.1; the total mass of the copolymer and N, Nv-bis(2-hydroxyethyl)decylamide to the second solvent is 1g:300mL.

[0132] (2) Cold water washing: The dyed polyester fabric obtained in step (1) is cold-washed for 10 minutes at a bath ratio of 1:20, and then dehydrated.

[0133] (3) Padding color fixing agent: The polyester fabric is immersed in the padding working solution for dipping and padding, and the liquid carrying rate is 70%.

[0134] Padding working fluid formula: 45 parts of epoxy compound, 7 parts of cationic compound, and 20 parts of deionized water.

[0135] The epoxy compound is a mixture of polyethylene glycol glycidyl ether and epichlorohydrin in a mass ratio of 1:1.

[0136] The cationic compound is 2,3-epoxypropyltrimethylammonium chloride.

[0137] (4) Heat treatment: The impregnated polyester fabric was heated to 90°C at a rate of 1°C / min for 20 min.

[0138] (5) Shaping: The heat-treated polyester fabric is shaped at a temperature of 200°C.

[0139] Example 2

[0140] A short-process polyester color fixing process comprises the following steps:

[0141] (1) Dyeing: The polyester fabric is immersed in a dye bath for dyeing at a bath ratio of 1:20, a temperature of 100°C, and a time of 40 minutes. After dyeing, the dye bath is cooled to 60°C, and alkali is added to adjust the pH value to 11. The temperature is kept for 15 minutes to allow the polymer leveling agent to be fully hydrolyzed, and then the water is drained.

[0142] The dye bath formula is as follows: CI Disperse Red 177 2% (owf), polymer leveling agent 1.5 g / L, glacial acetic acid 1 g / L.

[0143] The preparation method of the polymer leveling agent is as follows:

[0144] S1: 3-methacrylamidophenylboronic acid and a hydrophilic monomer were mixed in DMF, 4,4-azo(4-cyanovaleric acid) was added under nitrogen protection and reacted at 120°C for 2h, the obtained reaction solution was poured into twice the volume of water for precipitation, the precipitate was filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a copolymer;

[0145] The hydrophilic monomer is a mixture of acrylic acid and dimethylaminoethyl methacrylate in a molar ratio of 2:1.

[0146] The molar ratio of the phenylboronic acid monomer to the total molar ratio of the hydrophilic monomer is 1:4; the added amount of the initiator is 3% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

[0147] S2: After the copolymer and N, N-bis(2-hydroxyethyl)decylamide are mixed in ethylene glycol, NaOH is added to adjust the pH of the reaction solution to 9, and then the reaction is stirred at room temperature for 30 minutes. The obtained reaction solution is poured into twice the volume of water for precipitation, and the precipitate is filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a polymer leveling agent.

[0148] The molar ratio of the phenylboronic acid groups in the copolymer to the molar ratio of N, N-bis(2-hydroxyethyl)decylamide is 1:1.05; the total mass of the copolymer and N, N-bis(2-hydroxyethyl)decylamide to the second solvent is 1 g:400 mL.

[0149] (2) Cold water washing: The dyed polyester fabric obtained in step (1) is cold-washed for 10 minutes at a bath ratio of 1:20, and then dehydrated.

[0150] (3) Padding color fixing agent: The polyester fabric is immersed in the padding working solution for dipping and padding, and the liquid carrying rate is 70%.

[0151] Padding working fluid formula: 45 parts of epoxy compound, 7 parts of cationic compound, and 20 parts of deionized water.

[0152] The epoxy compound is a mixture of polyethylene glycol glycidyl ether and epichlorohydrin in a mass ratio of 1:1.

[0153] The cationic compound is 2,3-epoxypropyltrimethylammonium chloride.

[0154] (4) Heat treatment: The impregnated polyester fabric was heated to 80°C at a rate of 2°C / min for 30 min.

[0155] (5) Shaping: The heat-treated polyester fabric is shaped at a temperature of 180°C.

[0156] Example 3

[0157] A short-process polyester color fixing process comprises the following steps:

[0158] (1) Dyeing: The polyester fabric is immersed in a dye bath for dyeing at a bath ratio of 1:10, a temperature of 140°C, and a time of 20 min. After dyeing, the dye bath is cooled to 80°C, and alkali is added to adjust the pH value to 10. The temperature is kept at this temperature for 30 min to allow the polymer leveling agent to be fully hydrolyzed, and then the water is drained.

[0159] The dye bath formula is as follows: CI Disperse Red 1772% (owf), polymer leveling agent 1.5 g / L, glacial acetic acid 1 g / L.

[0160] The preparation method of the polymer leveling agent is as follows:

[0161] S1: 3-Acrylamidophenylboronic acid and a hydrophilic monomer were mixed in DMSO, and azobisisoheptanenitrile was added under nitrogen protection to react at 80°C for 6 hours. The obtained reaction solution was poured into twice the volume of water for precipitation, and the precipitate was filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a copolymer;

[0162] The hydrophilic monomer is a mixture of methacrylic acid and hydroxypropyl methacrylate in a ratio of 1:1.

[0163] The molar ratio of the phenylboronic acid monomer to the total molar ratio of the hydrophilic monomer is 1:3; the added amount of the initiator is 1% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

[0164] S2: After the copolymer and N, N-bis(2-hydroxyethyl)decylamide are mixed in methanol, NaOH is added to adjust the pH of the reaction solution to 9, and then the reaction is stirred at room temperature for 30 minutes. The obtained reaction solution is poured into twice the volume of water for precipitation, and the precipitate is filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a polymer leveling agent.

[0165] The molar ratio of the phenylboronic acid group in the copolymer to the molar ratio of N, N-bis(2-hydroxyethyl)decylamide is 1:1.2; the total mass of the copolymer and N, N-bis(2-hydroxyethyl)decylamide to the second solvent is 1 g:200 mL.

[0166] (2) Cold water washing: The dyed polyester fabric obtained in step (1) is cold-washed for 10 minutes at a bath ratio of 1:20, and then dehydrated.

[0167] (3) Padding color fixing agent: The polyester fabric is immersed in the padding working solution for double dipping and double padding, and the liquid carrying rate is 70%.

[0168] Padding working fluid formula: 45 parts of epoxy compound, 7 parts of cationic compound, and 20 parts of deionized water.

[0169] The epoxy compound is a mixture of polyethylene glycol glycidyl ether and epichlorohydrin in a mass ratio of 1:1.

[0170] The cationic compound is 2,3-epoxypropyltrimethylammonium chloride.

[0171] (4) Heat treatment: The impregnated polyester fabric was heated to 100°C at a rate of 1°C / min for 20 min.

[0172] (5) Shaping: The heat-treated polyester fabric is shaped at a temperature of 220°C.

[0173] Example 4

[0174] The difference from Example 1 is that the preparation method of the polymer dyeing accelerator is as follows:

[0175] S1: 3-Acrylamidophenylboronic acid and a hydrophilic monomer were mixed in DMAc, AIBN was added under nitrogen protection and reacted at 120°C for 4 h, the obtained reaction solution was poured into twice the volume of water for precipitation, the precipitate was filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a copolymer;

[0176] The hydrophilic monomer is a mixture of methacrylic acid and hydroxyethyl methacrylate in a molar ratio of 1:3.

[0177] The molar ratio of the phenylboronic acid monomer to the total molar ratio of the hydrophilic monomer is 1:5; the added amount of the initiator is 2% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

[0178] S2: After the copolymer and N, N-bis(2-hydroxyethyl)decylamide are mixed in methanol, NaOH is added to adjust the pH of the reaction solution to 9, and then the reaction is stirred at room temperature for 30 minutes. The obtained reaction solution is poured into twice the volume of water for precipitation, and the precipitate is filtered and washed with deionized water for 3 times, and dried at 80°C to constant weight to obtain a polymer leveling agent.

[0179] The molar ratio of the phenylboronic acid group in the copolymer to the molar ratio of N, N-bis(2-hydroxyethyl)decylamide is 1:1.1; the total mass of the copolymer and N, N-bis(2-hydroxyethyl)decylamide to the second solvent is 1 g:300 mL.

[0180] Example 5

[0181] The difference from Example 1 is that N, N-bis (2-hydroxyethyl) decylamide in the preparation of the polymer dyeing accelerator is replaced by N, N-bis (2-hydroxyethyl) octylamide.

[0182] Example 6

[0183] The difference from Example 1 is that N, N-bis (2-hydroxyethyl) decylamide in the preparation of the polymer dyeing accelerator is replaced by N, N-bis (2-hydroxyethyl) dodecylamide.

[0184] Example 7

[0185] The difference from Example 1 is that the formula of the dye bath is as follows: CI Disperse Red 1772% (owf), polymer leveling agent 1 g / L, and glacial acetic acid 1 g / L.

[0186] Example 8

[0187] The difference from Example 1 is that the formula of the dye bath is as follows: CI Disperse Red 1772% (owf), polymer leveling agent 2 g / L, and glacial acetic acid 1 g / L.

[0188] Example 9

[0189] The difference from Example 1 is that the liquid carrying rate in step (3) is 60%.

[0190] Example 10

[0191] The difference from Example 1 is that the liquid carrying rate in step (3) is 80%.

[0192] Embodiment 11

[0193] The difference from Example 1 is that the reinforcement working solution in step (3) is formulated as follows: 40 parts of pentaerythritol glycidyl ether, 4 parts of 3-chloro-2-hydroxypropyltrimethylammonium chloride, 10 parts of polyether polyol, and 15 parts of deionized water.

[0194] Example 12

[0195] The difference from Example 1 is that the reinforcement working solution in step (3) is formulated as follows: 50 parts of epoxy compound, 10 parts of 2,3-epoxypropyltrimethylammonium chloride, 2 parts of polyether polyol, and 30 parts of deionized water.

[0196] The epoxy compound is a mixture of epichlorohydrin and glycidol in a mass ratio of 1:1.

[0197] Comparative Example 1

[0198] The difference from Example 1 is that the copolymer prepared in Example 1 is used as the dyeing accelerator instead of the polymer dyeing accelerator, that is, the dyeing bath formula is as follows: CI Disperse Red 1772% (o.Wf), Example 1 copolymer 1.5 g / L, glacial acetic acid 1 g / L.

[0199] Comparative Example 2

[0200] The difference from Example 1 is that N, N-bis (2-hydroxyethyl) decanamide is used as the accelerator of the dye bath instead of the polymer accelerator, that is, the dye bath formula is as follows: CI Disperse Red 1772% (owf), N, N-bis (2-hydroxyethyl) decanamide 1.5 g / L, and glacial acetic acid 1 g / L.

[0201] Comparative Example 3

[0202] The difference from Example 1 is that no dye accelerator is added to the dye bath, that is, the dye bath formula is as follows: CI Disperse Red 1772% (o.wf), glacial acetic acid 1 g / L.

[0203] Comparative Example 4

[0204] The difference from Example 1 is that no dyeing accelerator is added to the dye bath in step (1) and the formula of the padding working solution in step (3) is as follows: 45 parts of epoxy compound, 7 parts of cationic compound, 20 parts of polyether polyol, and 20 parts of deionized water; the types of epoxy compound and cationic compound are the same as in Example 1.

[0205] The molecular structures of the copolymers prepared in Examples 1 to 4 were characterized by the following methods (1) and (2):

[0206] (1) The unit composition of the copolymer was analyzed by hydrogen nuclear magnetic spectrum. The solvent was deuterated ethanol. The composition of the repeating unit, that is, the ratio of x to y, could be analyzed by hydrogen spectrum.

[0207] (2) Gel chromatography (GPC) is used to analyze the molecular weight of the copolymer. The value of x can be calculated based on the number average molecular weight and the repeating unit.

[0208] The molecular structure information of the copolymers prepared in Examples 1 to 4 is listed in Table 1. The H NMR spectrum of the copolymer prepared in Example 1 is shown in the appendix of the specification. Figure 1 From the analysis in the figure, we can see that the positions at 7-8ppm and 3.51ppm correspond to the benzene ring proton peak and methylene proton peak of the phenylboronic acid unit and hydroxyethyl methacrylate unit, respectively. By comparing the relationship between the peak area and the number of protons, we can find that the minimum repeating unit is a combination of phenylboronic acid unit (x) and hydroxyethyl methacrylate (y) units with a ratio of 1:3.

[0209] Table 1

[0210]

[0211]

[0212] The H NMR spectrum of the polymer dyeing accelerator prepared in Example 1 is shown in the attached manual. Figure 1From the figure, we can see that the absorption peak of the benzene ring on the phenylboronic acid unit shifts, and the proton peak of the methylene group on the diethanolamine monomer appears, indicating that the diethanolamine monomer is successfully grafted onto the side chain of the copolymer.

[0213] In order to study the pH responsiveness of the polymer dyeing accelerator, the polymer dyeing accelerator prepared in Example 1 and the product obtained by hydrolysis of the polymer dyeing accelerator under alkaline conditions were analyzed by nuclear magnetic hydrogen spectrum. The polymer dyeing accelerator was dissolved in deuterated ethanol, and acetic acid was added to adjust the pH to 4.5 to obtain a sample to be tested under weakly acidic conditions (simulated dye bath); the polymer dyeing accelerator was dissolved in deuterated ethanol, and NaOH was added to adjust the pH to 10 to obtain a sample to be tested under alkaline conditions (simulated alkaline hydrolysis). The nuclear magnetic hydrogen spectra of the two samples to be tested are shown in the attached manual. Figure 2 As can be seen from the figure, the NMR hydrogen spectra of the sample under weak acidic conditions are almost the same as those of the polymer accelerator, indicating that the structure of the polymer accelerator is stable under this pH value; the position of the proton peak of the sample under alkaline conditions has changed significantly. Specifically, the -(N + The proton peak position of CH2CH2O)- moves to 3.39ppm and 3.62ppm, and the -OH proton peak appears at 4.79ppm, indicating the dissociation of the surface boron-nitrogen coordination bond; however, the benzene ring proton peak corresponding to 7.2-7.6ppm does not undergo a large displacement change, indicating that the boron of phenylboronic acid is still in a strong polar state. This is due to the polarization of the B atom by the hydroxide under alkaline conditions, which is also beneficial to improve the hydrophilicity of the main chain of the copolymer obtained by hydrolysis and accelerate the dissolution.

[0214] In order to study the dyeing accelerator of the polymer dyeing accelerator prepared in different embodiments for disperse dyes, the degree of plasticization of the polymer dyeing accelerator prepared in Examples 1 to 6 on polyester fibers was evaluated. The evaluation dimensions of the degree of plasticization include the swelling property of the fiber and the glass transition temperature of the polyester:

[0215] The polyester was put into a solution containing a dyeing accelerator with a concentration of 2 g / L, and heat-treated at 130°C for 1 hour. After being taken out, it was dried at 80°C for 6 hours to obtain a sample to be tested. Control 1 was a solution without adding a dyeing accelerator, and the dyeing accelerator of control 2 was wintergreen oil. A NiKonE200 optical microscope was used to observe and measure the diameter of the fiber before and after swelling. 10 fibers were selected for each sample, 10 test sections were selected for each fiber, and each test section was measured 10 times. Then, the average diameter of a certain sample was calculated, and the swelling degree = (average diameter of the fiber after swelling - average diameter of the untreated fiber) / average diameter of the untreated fiber. A NETZSCH 204C differential scanning calorimeter was used to measure the glass transition temperature T of the fiber before and after swelling. g The measurement was carried out with a heating rate of 10°C / min and a nitrogen atmosphere.

[0216] Swelling degree and glass transition temperature T g The results are listed in Table 2.

[0217] Table 2

[0218]

[0219] From the data in the table, it can be seen that after adding the accelerator, the swelling degree of polyester increases and the glass transition temperature T g Decrease, indicating that the plasticity of polyester fiber is enhanced; and the polymer dye accelerator provided by the present invention is better for the plasticizing effect of polyester relative to the commonly used swelling dye accelerator wintergreen oil. And from the perspective of control 1 and control 2, the hydrolyzate of the polymer dye accelerator of the present invention has a poor swelling and swelling effect on polyester, and it is necessary for the two to be combined and bonded before they have suitable hydrophilicity and similarity. Specifically, the hydrophilicity of the copolymer is too strong, and it is difficult to be oleophilic inside the polyester. Although the side group N, N-bis (2-hydroxyethyl) capric amide is hydrophobic, it does not have similar compatibility with the structure of polyester. In addition, it can be seen from the results that the carbon atom number of the alkyl chain in the diethanolamine monomer has a greater impact on the plasticizing effect of the polymer dye accelerator. As the alkyl chain is longer, the plasticizing effect shows an increase first and then a decrease. The reason is that when the number of carbon atoms is less, the hydrophilicity of the polymer dye accelerator is stronger, and the affinity for polyester decreases; when the number of carbon atoms is more, the hydrophobicity of the polymer dye accelerator is stronger, and the degree of dispersion in water is lower, it is easy to agglomerate, and it is difficult to immerse in the fiber interior.

[0220] In order to study the fixing effect of the process of the present invention on disperse dyes, the fabrics obtained in the examples and comparative examples were subjected to the following tests:

[0221] The polyester fabric before heat setting in the embodiment or comparative example was stripped, and the concentration of the stripping solution was measured to calculate the color fixation rate, specifically as follows: the polyester fabric before heat setting in the embodiment was boiled in DMSO at 130°C for 30 minutes, with a bath ratio of 1:300, and the stripping solution was combined twice to obtain a stripping solution, and the absorbance of the stripping solution was tested by an ultraviolet spectrophotometer, and the color fixation rate was calculated according to the volume of the stripping solution, the color fixation rate = 1-(stripping solution absorbance-blank group absorbance) ÷ blank group absorbance × 100%. The blank group refers to the polyester fabric before heat setting replaced by undyed polyester fabric, and the color fixation rates are listed in Table 3.

[0222] Table 3

[0223]

[0224]

[0225] From the data in the table, it can be seen that the embodiment has a higher fixation rate than the comparative example. The fixation effect in the process comes from two aspects. On the one hand, as the polymer dye accelerator is hydrolyzed and dissolved, the plasticity of the polyester is reduced, and the disperse dye is sealed inside the polyester; on the other hand, the hydrophobic diethanolamine monomer obtained by the hydrolysis of the polymer dye accelerator migrates to the fiber surface, and reacts with the epoxy group by heating to form a polymer film outside the fiber to prevent the floating color or thermal migration of the dye from dissolving, thereby achieving the fixation effect, thereby omitting the steps of reduction washing and soaping. Specifically, the polymer dye accelerator plasticizes the polyester during the dyeing stage, enters the fiber, increases the diffusion degree of the disperse dye inside the fiber, and increases the dyeing rate; after the dyeing is completed, the pH of the dye bath is adjusted to a strong alkaline, and under hydrothermal conditions, the polymer dye accelerator decomposes and migrates out from the fiber, the plasticizing and swelling effect disappears, the fiber plasticity decreases, and the disperse dye is blocked. Therefore, in Comparative Examples 1 and 3, since no diethanolamine monomer remains on the fiber surface, a polymer film cannot be obtained, resulting in the dissolution of disperse dyes; in Comparative Example 2, diethanolamine monomer is added to the dye bath. Since diethanolamine monomer has poor water solubility, it agglomerates and sinks in the dye bath, making it difficult to evenly cover the fiber surface. Therefore, the amount of film formed in the color fixing stage is small and the color fixing effect is poor; in Comparative Example 4, polyether polyol is added to the color fixing padding working solution. Although the color fixing effect is good, the color depth of the fabric is poor due to the absence of a dyeing accelerator.

[0226] The dyed fabric after cold water washing in step (2) of Example 1 was immersed in DMSO at room temperature for 15 minutes, and the liquid obtained after immersion was analyzed by nuclear magnetic resonance spectroscopy. The results are shown in the appendix of the specification. Figure 3 As can be seen from the figure, the characteristic proton peak of N, N-bis(2-hydroxyethyl)decylamide can be observed, indicating that N, N-bis(2-hydroxyethyl)decylamide obtained by hydrolysis of the polymer dye accelerator remains on the surface of the dyed fabric after washing. As one of the components of the color fixing agent, it undergoes a cross-linking reaction with the epoxy group in the color fixing auxiliary agent to form a cross-linked polymer film covering the surface of the fabric to achieve a color fixing effect.

[0227] The K / S value of the dyed polyester fabric obtained in the embodiment and the comparative example was measured: the apparent color depth K / S value of the blended fabric obtained in the embodiment and the comparative example was tested using a Datacolor 650 colorimeter. The D65 light source and a 10° viewing angle were selected to measure the K / S value at the maximum absorption wavelength of the dyed fabric. Ten points were randomly selected for each sample for measurement, and then the average value was calculated.

[0228] The color fastness of the dyed polyester fabrics obtained in the examples and comparative examples was tested: the color fastness to washing with soap of the dyed fabrics was tested according to GB / T 3921-2008 "Textiles - Tests for Color Fastness - Color Fastness to Washing with Soap"; the color fastness to rubbing of the dyed fabrics was tested according to GB / T 3920-2008 "Textiles - Tests for Color Fastness - Color Fastness to Rubbing".

[0229] Table 4

[0230]

[0231]

[0232] From the data in the table, it can be seen that the fabric prepared by the process of the present invention has a higher color depth and color fastness than the comparative example. Specifically, since neither the copolymer nor the diethanolamine monomer has dyeing accelerator properties, the color depth of comparative examples 1 and 2 is relatively low; comparative examples 1 and 3 do not have a color fixing polymer film, so the color fastness is relatively low; in comparative example 2, since the diethanolamine monomer cannot evenly cover the surface of the fabric after dyeing, a complete polymer film cannot be formed, resulting in low color fastness. In addition, from the comparison of the data of each embodiment, it can be seen that the higher the concentration of the polymer accelerator in the dye bath, the greater the color depth, the higher the liquid rate in the padding color fixing working solution, the higher the polyol, and the higher the color fastness.

[0233] The above contents are further detailed descriptions of the present invention in combination with specific preferred technical solutions, and it cannot be determined that the specific implementation of the present invention is limited to these descriptions. For professionals and technicians in the technical field to which the present invention belongs, several simple deductions or substitutions can be made without departing from the concept of the present invention, which should be regarded as belonging to the protection scope of the present invention.

Claims

1. A short-process polyester color fixing process, characterized in that: The following steps are involved: (1) Dyeing: Immerse the polyester fabric in a dye bath for dyeing; After dyeing, alkali is added to adjust the pH value to above 10 for hydrolysis reaction, and then drainage is conducted; the dye bath includes disperse dyes and polymer leveling agents; the formula of the dye bath includes: disperse dyes 1-2% owf, polymer leveling agents 1-2g / L, and glacial acetic acid 0.5-1.5g / L; (2) washing: washing the dyed polyester obtained in step (1); (3) a padding color fixing working solution, wherein the formula of the color fixing working solution includes: 40 to 50 parts of an epoxy compound, 4 to 10 parts of a cationic compound, 0 to 20 parts of a polyol, and 10 to 30 parts of deionized water; the epoxy compound is selected from at least one of epichlorohydrin, glycidol, pentaerythritol glycidyl ether, glycidyl ether, and polyethylene glycol diglycidyl ether; (4) Heat treatment; (5) Heat setting; The polymer leveling agent has the following molecular structure: In the formula, R1 and R2 are independently selected from H or CH3; R3 is selected from at least one of H, C2H4OH, C2H4N(CH3)2, C2H4N(C2H5)2, CH2CH(CH3)OH; R4 is selected from a straight-chain alkyl group having 7 to 11 carbon atoms; the ratio of x to y is 1:2 to 4, and the value of x is 3 to 15.

2. A short-process polyester color fixing process according to claim 1, characterized in that: The polyol in step (3) is selected from at least one of polyether polyol, triisopropanolamine, triethanolamine and pentaerythritol.

3. A short-process polyester color fixing process according to claim 1, characterized in that: The cationic compound in step (3) is selected from at least one of 3-chloro-2-hydroxypropyltrimethylammonium chloride and 2,3-epoxypropyltrimethylammonium chloride.

4. A short-process polyester color fixing process according to claim 1, characterized in that: The preparation method of the polymer leveling agent is as follows: S1: mixing phenylboronic acid monomer and hydrophilic monomer in a first solvent, adding an initiator to carry out polymerization reaction, and obtaining a copolymer; S2: The copolymer and the diethanolamine monomer are mixed in a second solvent and stirred under alkaline conditions to obtain a polymer leveling agent.

5. A short-process polyester color fixing process according to claim 4, characterized in that: The preparation method of the polymer leveling agent meets at least one of the following characteristics 1 to 6: Feature 1: The first solvent is at least one of N,N-dimethylformamide DMF, dimethyl sulfoxide DMSO, and N,N-dimethylacetamide DMAc; Feature 2: The phenylboronic acid monomer is 3-acrylamide phenylboronic acid or 3-methacrylamide phenylboronic acid; Feature 3: The hydrophilic monomer is selected from at least one of methacrylic acid, acrylic acid, hydroxyethyl methacrylate, hydroxyethyl acrylate, dimethylaminoethyl methacrylate, diethylaminoethyl methacrylate, and hydroxypropyl methacrylate; Feature 4: The initiator is selected from at least one of azobisisobutyronitrile, azobisisoheptanenitrile, dimethyl azobisisobutyrate, and 4,4-azo(4-cyanovaleric acid); Feature 5: The polymerization reaction is carried out in an inert atmosphere, the reaction temperature is 80-120°C, and the reaction time is 2-6 hours; Feature 6: The molar ratio of the phenylboronic acid monomer and the hydrophilic monomer is 1:1-5, and the amount of the initiator added is 1%-3% of the total mass of the phenylboronic acid monomer and the hydrophilic monomer.

6. A short-process polyester color fixing process according to claim 4, characterized in that: The preparation method of the polymer leveling agent meets at least one of the following characteristics 1 to 6: Feature 1: The diethanolamine monomer is selected from at least one of N,N-bis(2-hydroxyethyl)octanamide, N,N-bis(2-hydroxyethyl)nonanamide, N,N-bis(2-hydroxyethyl)decanamide, N,N-bis(2-hydroxyethyl)undecanamide and N,N-bis(2-hydroxyethyl)dodecanamide; Feature 2: The second solvent is at least one of methanol, ethanol, isopropanol, and ethylene glycol; Characteristic 3: Alkaline conditions refer to adding acid or base to adjust the reaction pH to 9 ± 0.5; Feature 4: Stirring reaction means stirring reaction at room temperature for 30 minutes; Characteristic 5: The ratio of the molar amount of phenylboronic acid groups in the copolymer to the molar amount of diethanolamine monomer is 1:1.05-1.2; Feature 6: The feeding ratio of the total mass of the copolymer and the diethanolamine monomer to the second solvent is 1g:200-400mL.

7. A short-process polyester color fixing process according to claim 1, characterized in that: The color fixing process meets at least one of the following characteristics 1 to 7: Feature 1: The dyeing temperature of step (1) is 100-140°C, the dyeing time is 20-40 min, and the bath ratio is (1:10-20); Feature 2: The hydrolysis reaction temperature of step (1) is 60-80°C and the time is 15-30 minutes; Feature 3: The water washing temperature in step (2) is room temperature, the water washing time is 10 to 20 minutes, and the bath ratio is (1:10 to 20); Feature 4: The dipping and rolling in step (3) is one dipping and one rolling or two dipping and two rolling; Feature 5: The padding liquid rate in step (3) is 60% to 80%; Feature 6: The heat treatment in step (4) is to heat the temperature to 80-100°C at a rate of 1-2°C / min for 20-30min; Feature 7: The heat setting temperature of step (5) is 180-220°C.

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