A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing or washing.
By combining disperse dye microcapsules and polyacrylic acid sizing agents, the dyeing process of polyester fabric was optimized, achieving desizing and washing-free operation. This solved the problems of difficult polyester dyeing and water consumption, and yielded polyester fabrics with high color fastness and abrasion and light resistance.
Patent Information
- Application Number
- CN202311094116.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2023-08-29
- Publication Date
- 2025-11-11
- Estimated Expiration
- 2043-08-29
AI Technical Summary
The polyester dyeing process requires desizing, which leads to a large consumption of water resources and pollution. Dyeing is also difficult, and existing technologies cannot achieve an environmentally friendly and energy-saving dyeing process.
By employing a combination of disperse dye microcapsules, polyacrylic sizing agents, defoamers, and surfactants, and optimizing the dyeing process, desizing and washing are eliminated. The microcapsules rupture at high temperatures to release the dye, and the combined effect of the polyacrylic sizing agents and defoamers improves the color fastness and uniformity of the dyeing process.
It enables waterless dyeing of polyester fabrics, with uniform dyeing effect, high color fastness, and resistance to abrasion and light, reducing water consumption and production costs, and improving dyeing efficiency.
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Figure BDA0004418594030000091 
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Abstract
Description
Technical Field
[0001] This invention relates to the technical field of textile printing and dyeing, and in particular to a dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing. Background Technology
[0002] Polyester, also known as polyester fiber, is a synthetic fiber obtained by spinning polyester, which is formed by the condensation polymerization of organic diacids and diols. It is currently the most widely used synthetic fiber in the world. Due to its high degree of polymerization, large molecular weight, and compact structure, it possesses excellent wrinkle resistance and shape retention, high strength and elastic recovery, durability, wrinkle-resistant and non-sticky properties, and is widely used. However, the high degree of polymerization, large molecular weight, and compact structure of polyester make it difficult for small dye molecules to penetrate into the polyester molecule. The lack of reactive groups within the molecule makes dyeing polyester difficult. Currently, common methods for dyeing polyester include: high temperature and high pressure method (130℃, 2kg / cm²). 2 The dye molecules are applied by baking under pressure or by hot melting (around 180-220℃) to allow the dye molecules to penetrate into the fiber and be dyed.
[0003] In the polyester dyeing process, the greige fabric needs to be desized first to thoroughly clean the surface of the fabric, removing all sizing agents and impurities before finishing and dyeing. Subsequent cleaning requires large amounts of caustic soda, sodium hydrosulfite, reducing agents, and water to achieve good colorfastness. This process generates a significant amount of desizing wastewater, resulting in high wastewater treatment costs and external discharge pressure. Dyeing one ton of polyester fabric requires nearly 40 tons of water, consuming considerable water and energy. With increasingly stringent national regulations on environmental protection in the dyeing and printing industry, energy conservation and emission reduction have become crucial for the industry's long-term development. Therefore, optimizing the dyeing process for polyester fabric and researching more environmentally friendly and energy-efficient dyeing techniques is imperative. Summary of the Invention
[0004] To address the aforementioned technical problems, this invention provides a dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing. By optimizing the dyeing process, the method achieves the goal of eliminating the need for washing and can produce polyester fabrics with uniform dyeing effect, high color fastness, abrasion resistance, and light resistance.
[0005] The specific technical solution of this invention is: a dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing, comprising the following steps:
[0006] Step 1, Dyeing paste: Mix disperse dye microcapsules, polyacrylic slurry, defoamer, surfactant and water evenly, adjust the pH to 5-6 to obtain dyeing paste; the wall material of the disperse dye microcapsules is polyurethane and acid-hydrolyzed modified starch, and the core material is disperse dye, glucono-delta-lactone and calcium carbonate;
[0007] Step 2, dyeing: Immerse the polyester fabric in dyeing paste to obtain dyed polyester;
[0008] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried, baked and set in sequence to obtain wear-resistant and light-resistant polyester fabric.
[0009] This invention uses lightweight and non-stretchable polyester fabric as the base fabric and disperse dye microcapsules, polyacrylic acid sizing agents, defoamers, surfactants and water as modified sizing agents to achieve the purpose of waterless washing. Furthermore, by optimizing the dyeing process, a polyester fabric with uniform dyeing effect, high color fastness, abrasion resistance, and light resistance has been developed. After dyeing, the fabric can be directly produced without desizing and washing.
[0010] Disperse dye microcapsules can release disperse dyes by rupturing the wall material during the dyeing process. Combined with the synergistic effect of polyacrylic sizing agents, defoamers, and surfactants, they can improve the color fastness of dyeing. Moreover, in the subsequent pre-baking and baking processes, they can not only enable the dye to develop color and further improve the color fastness of dyeing, but also decompose and remove trace amounts of residual microcapsules, achieving the purpose of waterless washing.
[0011] Preferably, the method for preparing the disperse dye microcapsules includes the following steps:
[0012] (1) Starch is added to water to make starch slurry, then sulfuric acid is added for acid hydrolysis, the pH is adjusted to 3.5-5, and then after post-treatment, acid hydrolyzed modified starch is obtained.
[0013] (2) Glucose lactone, calcium carbonate and n-octanol were wet ball milled and then filtered to obtain modified calcium carbonate.
[0014] (3) After adding disperse dye and modified calcium carbonate to water and stirring, adjust the pH to 4-6, add a mixture of amine resin prepolymer and acid-hydrolyzed modified starch I to carry out a preliminary reaction; add a mixture of methyl methacrylate and ammonium persulfate II to carry out a second reaction, let it stand to precipitate, add ammonia water to neutralize, and then filter to obtain disperse dye microcapsules.
[0015] Disperse dye microcapsules can release disperse dyes during the dyeing process by controlling the dyeing conditions. Due to the good affinity between the wall material and polyester, the dye can settle on the fiber surface. The high-temperature treatment during dyeing causes the wall material to rupture, slowly releasing the disperse dye. Simultaneously, the acid-hydrolyzed modified starch in the wall material acts as a thickener and adsorbent, ensuring the disperse dye is firmly adsorbed onto the polyester surface. Furthermore, the starch, after acid hydrolysis, produces dextrins with smaller molecular weights, which can better bind to the wall material, resulting in high binding stability.
[0016] The core material of the microcapsules also incorporates modified calcium carbonate, which, after wet ball milling with glucono-delta-lactone and n-octanol, forms a coating layer on the surface composed of glucono-delta-lactone and n-octanol. By controlling the amount added, the oily liquid n-octanol forms another coating layer on the outermost layer, thus preventing premature reaction between glucono-delta-lactone and calcium carbonate in subsequent reactions. During the dyeing process, n-octanol is more volatile at high temperatures, and glucono-delta-lactone is more easily exposed to water and hydrolyzed under these conditions. Calcium carbonate also generates bubbles under acidic and high-temperature conditions. These bubbles help promote the diffusion of dispersed dyes within the microcapsules, improve dispersibility, and facilitate dye penetration into the interior of the synthetic fiber, thereby increasing dye uptake and color fastness, and improving dyeing efficiency.
[0017] Preferably, in step (1), the mass concentration of the starch slurry is 35-40%; the amount of sulfuric acid added is 5-8% of the starch slurry; and the acid hydrolysis is carried out at 40-45°C for 70-80 minutes.
[0018] Preferably, in step (2), the mass ratio of gluconolactone, calcium carbonate and n-octanol is 3-4:1:10; the particle size of calcium carbonate is 20-100 nm; and the wet ball milling speed is 200-300 rpm and the time is 20-30 min.
[0019] Calcium gluconate, obtained from the decomposition of gluconolactone, can not only provide an acidic environment for calcium carbonate, but also chelate with calcium ions. Calcium gluconate can also act as a dispersant to promote the dispersion of dyes.
[0020] Preferably, in step (3), the mass ratio of the disperse dye, modified calcium carbonate, and water is 1:4 to 6:150; the amount of melamine resin prepolymer added is 3 to 4 times the mass of the disperse dye; the mass ratio of the melamine resin prepolymer to the acid-hydrolyzed modified starch is 1:0.2 to 0.3; the amount of methyl methacrylate added is 1 to 1.5 times the mass of the disperse dye; the mass ratio of methyl methacrylate to ammonium persulfate is 1:0.1 to 0.2; the preliminary reaction is carried out at 50 to 60°C for 1 to 2 hours; and the secondary reaction is carried out at 70 to 75°C for 1 to 1.5 hours.
[0021] Preferably, the ratio of the disperse dye microcapsules, polyacrylic acid slurry, defoamer, surfactant and water is 5-9g: 3-4g: 0.5-0.8g: 0.2-0.6g: 1L.
[0022] Preferably, the polyacrylic slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
[0023] Polyacrylic acid pastes have thickening and dispersing properties, which can prevent dye migration, improve dye leveling, and also disperse and chelate calcium and magnesium ions in water, softening the water and reducing the impact of metal ions on dyeing.
[0024] Preferably, the defoamer is one or more of a high-carbon alcohol fatty acid ester complex, polydimethylsiloxane, and emulsified silicone oil; the surfactant is one or more of glyceryl monostearate, lauryl alcohol polyoxyethylene ether, sodium dodecylbenzenesulfonate, sodium glycocholate, and polysorbate.
[0025] Defoamers have a defoaming effect and can improve the dyeing effect.
[0026] Preferably, the staining process involves first heating the sample to room temperature at a rate of 3–4 °C / min, then maintaining the temperature at 130–140 °C for 20–30 min, and finally cooling the sample to room temperature at a rate of -4–-2 °C / min, with a pH of 4–6 and a bath ratio of 1:5–10.
[0027] Preferably, the pre-drying is carried out at a temperature of 110-120°C with hot air for 2-3 minutes; the baking temperature is 200-210°C and the time is 120-150 seconds.
[0028] Compared with the prior art, the present invention has the following advantages:
[0029] (1) This invention uses a lightweight and non-stretchable polyester fabric as the base fabric, and uses disperse dye microcapsules, polyacrylic acid sizing agents, defoamers, surfactants and water as modified sizing agents to achieve the purpose of waterless washing. Furthermore, by optimizing the dyeing process, a polyester fabric with uniform dyeing effect, high color fastness, abrasion resistance and light resistance can be produced directly after dyeing without desizing and washing.
[0030] (2) Disperse dye microcapsules can release disperse dyes by breaking the wall material during the dyeing process. This not only enhances the affinity and adsorption strength of disperse dyes on the polyester surface, but also facilitates the dye to penetrate into the interior of the chemical fiber, thereby increasing the dyeing rate and color fastness and improving the dyeing efficiency.
[0031] (3) The subsequent pre-drying and baking processes can not only make the dye develop color and further improve the color fastness of the dyeing, but also decompose and remove trace amounts of residual microcapsules, achieving the purpose of water-free washing. Detailed Implementation
[0032] The present invention will be further described below with reference to embodiments.
[0033] A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing includes the following steps:
[0034] Step 1, Dyeing Paste: Mix 5-9g: 3-4g: 0.5-0.8g: 0.2-0.6g: 1L of disperse dye microcapsules, polyacrylic acid slurry, defoamer, surfactant, and water until homogeneous. Adjust the pH to 5-6 to obtain the dyeing paste. The polyacrylic acid slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate. The defoamer is one or more of the following: higher alcohol fatty acid ester complex, polydimethylsiloxane, and emulsified silicone oil. The surfactant is one or more of the following: glyceryl monostearate, lauryl alcohol polyoxyethylene ether, sodium dodecylbenzenesulfonate, sodium glycocholate, and polysorbate.
[0035] The preparation method of disperse dye microcapsules includes the following steps:
[0036] (1) Add starch to water to prepare a starch slurry with a mass concentration of 35-40%, then add sulfuric acid and acid hydrolyze at 40-45℃ for 70-80 minutes. The amount of sulfuric acid added is 5-8% of the starch slurry. Adjust the pH to 3.5-5.0. After post-treatment, acid hydrolyzed modified starch is obtained.
[0037] (2) Glucose lactone, calcium carbonate (particle size 20-100nm) and n-octanol were mixed in a mass ratio of 3-4:1:10 and then wet ball milled at a speed of 200-300 rpm for 20-30 min. After filtration, modified calcium carbonate was obtained.
[0038] (3) Disperse dye and modified calcium carbonate are added to water in a mass ratio of 1:4 to 6:150. After stirring, the pH is adjusted to 4 to 6. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.2 to 0.3 is added dropwise, wherein the amount of melamine resin prepolymer added is 3 to 4 times the mass of disperse dye. The mixture is reacted at 50 to 60°C for 1 to 2 hours. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.1 to 0.2 is added dropwise, wherein the amount of methyl methacrylate added is 1 to 1.5 times the mass of disperse dye. The mixture is reacted at 70 to 75°C for 1 to 1.5 hours. The mixture is allowed to stand and precipitate. Ammonia water is added to neutralize the precipitate. After filtration, disperse dye microcapsules are obtained.
[0039] The preparation method of the melamine resin prepolymer is as follows: water and 37wt% formaldehyde aqueous solution are mixed in a mass ratio of 2:1 and stirred evenly. Sodium hydroxide solution is added to adjust the pH to 8, and then 16% melamine by mass of water is added. After stirring evenly, the mixture is reacted at 80℃ for 0.5h. After cooling, the melamine resin prepolymer is obtained.
[0040] Step 2, dyeing: Immerse the polyester fabric in the dyeing paste for dyeing. First, heat the fabric from room temperature at a rate of 3-4℃ / min, then keep it at 130-140℃ for 20-30 minutes, and then cool it down to room temperature at a rate of -4--2℃ / min. The pH is 4-6 and the liquor ratio is 1:5-10 to obtain dyed polyester.
[0041] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried (at a temperature of 110-120℃, hot air pre-drying for 2-3 minutes), baked (at a temperature of 200-210℃, for 120-150 seconds) and set in sequence to obtain abrasion-resistant and light-resistant polyester fabric.
[0042] Example 1
[0043] A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing includes the following steps:
[0044] Step 1, Dyeing Paste: Mix 7g:3g:0.6g:0.4g:1L of disperse dye microcapsules, polyacrylic acid slurry, defoamer (higher alcohol fatty acid ester complex), surfactant (lauryl alcohol polyoxyethylene ether, sodium dodecylbenzene sulfonate), and water until homogeneous. Adjust the pH to 5-6 to obtain the dyeing paste. The polyacrylic acid slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
[0045] The preparation method of disperse dye microcapsules includes the following steps:
[0046] (1) Add starch to water to prepare a starch slurry with a mass concentration of 35%, then add sulfuric acid and acid hydrolyze at 45°C for 70 min. The amount of sulfuric acid added is 7% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0047] (2) Glucose lactone, calcium carbonate (average particle size of 50 nm) and n-octanol were mixed in a mass ratio of 4:1:10 and then wet ball milled at a speed of 200 rpm for 30 min. After filtration, modified calcium carbonate was obtained.
[0048] (3) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:5:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.25 was added dropwise, with the amount of melamine resin prepolymer being 3.3 times the mass of disperse dye. The mixture was reacted at 55°C for 2 hours. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.2 times the mass of disperse dye. The mixture was reacted at 70°C for 1.5 hours, allowed to stand and precipitate, neutralized with ammonia water, and then filtered to obtain disperse dye microcapsules.
[0049] Step 2, dyeing: Immerse the polyester fabric in the dyeing paste for dyeing. First, heat the fabric from room temperature at a rate of 4℃ / min, then keep it at 135℃ for 25min, and then cool it down to room temperature at a rate of -3℃ / min. The pH is 4-6 and the liquor ratio is 1:8 to obtain dyed polyester.
[0050] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried (at 120℃, hot air pre-drying for 3 minutes), baked (at 210℃ for 150 seconds) and set in sequence to obtain abrasion-resistant and light-resistant polyester fabric.
[0051] Example 2
[0052] A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing includes the following steps:
[0053] Step 1, Dyeing Paste: Mix 7g:3g:0.6g:0.4g:1L of disperse dye microcapsules, polyacrylic acid slurry, defoamer (higher alcohol fatty acid ester complex), surfactant (lauryl alcohol polyoxyethylene ether, sodium dodecylbenzene sulfonate), and water until homogeneous. Adjust the pH to 5-6 to obtain the dyeing paste. The polyacrylic acid slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
[0054] The preparation method of disperse dye microcapsules includes the following steps:
[0055] (1) Add starch to water to prepare a starch slurry with a mass concentration of 40%, then add sulfuric acid and acid hydrolyze at 45°C for 80 minutes. The amount of sulfuric acid added is 8% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0056] (2) Glucose lactone, calcium carbonate (average particle size of 40 nm) and n-octanol were mixed in a mass ratio of 4:1:10 and then wet-milled at 300 rpm for 30 min. After filtration, modified calcium carbonate was obtained.
[0057] (3) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:4:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.2 was added dropwise, with the amount of melamine resin prepolymer being 3 times the mass of disperse dye. The mixture was reacted at 60°C for 1.5 h. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.5 times the mass of disperse dye. The mixture was reacted at 75°C for 1.5 h. After settling, ammonia water was added to neutralize the sediment. After filtration, disperse dye microcapsules were obtained.
[0058] Step 2, dyeing: Immerse the polyester fabric in the dyeing paste for dyeing. First, heat the fabric from room temperature at a rate of 4℃ / min, then keep it at 135℃ for 25min, and then cool it down to room temperature at a rate of -3℃ / min. The pH is 4-6 and the liquor ratio is 1:8 to obtain dyed polyester.
[0059] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried (at 120℃, hot air pre-drying for 3 minutes), baked (at 210℃ for 150 seconds) and set in sequence to obtain abrasion-resistant and light-resistant polyester fabric.
[0060] Example 3
[0061] A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing includes the following steps:
[0062] Step 1, Dyeing Paste: Mix 7g:3g:0.6g:0.4g:1L of disperse dye microcapsules, polyacrylic acid slurry, defoamer (higher alcohol fatty acid ester complex), surfactant (lauryl alcohol polyoxyethylene ether, sodium dodecylbenzene sulfonate), and water until homogeneous. Adjust the pH to 5-6 to obtain the dyeing paste. The polyacrylic acid slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
[0063] The preparation method of disperse dye microcapsules includes the following steps:
[0064] (1) Add starch to water to prepare a starch slurry with a mass concentration of 35%, then add sulfuric acid and acid hydrolyze at 40°C for 80 min. The amount of sulfuric acid added is 5% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0065] (2) Glucose lactone, calcium carbonate (average particle size of 50 nm) and n-octanol were mixed in a mass ratio of 3:1:10 and then wet ball milled at 300 rpm for 20 min. After filtration, modified calcium carbonate was obtained.
[0066] (3) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:6:150. After stirring, the pH was adjusted to 5-6. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.3 was added dropwise, with the amount of melamine resin prepolymer being 4 times the mass of disperse dye. The mixture was reacted at 60°C for 2 hours. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.3 times the mass of disperse dye. The mixture was reacted at 72°C for 1.5 hours. The mixture was allowed to stand and precipitate. Ammonia water was added to neutralize the precipitate. After filtration, disperse dye microcapsules were obtained.
[0067] Step 2, dyeing: Immerse the polyester fabric in the dyeing paste for dyeing. First, heat the fabric from room temperature at a rate of 4℃ / min, then keep it at 135℃ for 25min, and then cool it down to room temperature at a rate of -3℃ / min. The pH is 4-6 and the liquor ratio is 1:8 to obtain dyed polyester.
[0068] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried (at 120℃, hot air pre-drying for 3 minutes), baked (at 210℃ for 150 seconds) and set in sequence to obtain abrasion-resistant and light-resistant polyester fabric.
[0069] Example 4
[0070] A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing includes the following steps:
[0071] Step 1, Dyeing Paste: Mix 9g:4g:0.8g:0.5g:1L of disperse dye microcapsules, polyacrylic acid slurry, defoamer (high carbon alcohol fatty acid ester complex), surfactant (lauryl alcohol polyoxyethylene ether, sodium dodecylbenzene sulfonate), and water until homogeneous. Adjust the pH to 5-6 to obtain the dyeing paste. The polyacrylic acid slurry is an emulsion slurry obtained by crosslinking polymerization of acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
[0072] The preparation method of disperse dye microcapsules includes the following steps:
[0073] (1) Add starch to water to prepare a starch slurry with a mass concentration of 35%, then add sulfuric acid and acid hydrolyze at 45°C for 70 min. The amount of sulfuric acid added is 7% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0074] (2) Glucose lactone, calcium carbonate (average particle size of 50 nm) and n-octanol were mixed in a mass ratio of 4:1:10 and then wet ball milled at a speed of 200 rpm for 30 min. After filtration, modified calcium carbonate was obtained.
[0075] (3) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:5:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.25 was added dropwise, with the amount of melamine resin prepolymer being 3.3 times the mass of disperse dye. The mixture was reacted at 55°C for 2 hours. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.2 times the mass of disperse dye. The mixture was reacted at 70°C for 1.5 hours, allowed to stand and precipitate, neutralized with ammonia water, and then filtered to obtain disperse dye microcapsules.
[0076] Step 2, dyeing: Immerse the polyester fabric in the dyeing paste for dyeing. First, heat the fabric from room temperature at a rate of 3℃ / min, then keep it at 130℃ for 30min, and then cool it down to room temperature at a rate of -4℃ / min. The pH is 4-6 and the liquor ratio is 1:8 to obtain dyed polyester.
[0077] Step 3, Post-dyeing treatment: The dyed polyester is pre-dried (at 110℃, hot air pre-drying for 3 minutes), baked (at 210℃ for 120 seconds) and set in sequence to obtain wear-resistant and light-resistant polyester fabric.
[0078] Comparative Example 1
[0079] The difference from Example 2 is that modified calcium carbonate is not added in the preparation method of disperse dye microcapsules.
[0080] The preparation method of disperse dye microcapsules includes the following steps:
[0081] (1) Add starch to water to prepare a starch slurry with a mass concentration of 40%, then add sulfuric acid and acid hydrolyze at 45°C for 80 minutes. The amount of sulfuric acid added is 8% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0082] (2) Disperse dye was added to water at a mass ratio of 1:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch at a mass ratio of 1:0.2 was added dropwise, with the amount of melamine resin prepolymer being 3 times the mass of disperse dye. The mixture was reacted at 60°C for 1.5 h. A mixture of methyl methacrylate and ammonium persulfate at a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.5 times the mass of disperse dye. The mixture was reacted at 75°C for 1.5 h. After settling, ammonia water was added to neutralize the precipitate. After filtration, disperse dye microcapsules were obtained.
[0083] Comparative Example 2
[0084] The difference from Example 2 is that the amount of gluconolactone added in the preparation method of disperse dye microcapsules is too small and the parameters of wet ball milling are different.
[0085] The preparation method of disperse dye microcapsules includes the following steps:
[0086] (1) Add starch to water to prepare a starch slurry with a mass concentration of 40%, then add sulfuric acid and acid hydrolyze at 45°C for 80 minutes. The amount of sulfuric acid added is 8% of the starch slurry. After acid hydrolysis, adjust the pH to 4.5-5. Then, after concentration, dehydration and drying, acid hydrolyzed modified starch is obtained.
[0087] (2) Glucose lactone, calcium carbonate (average particle size of 40 nm) and n-octanol were mixed in a mass ratio of 2:1:10 and then wet ball milled at 300 rpm for 15 min. After filtration, modified calcium carbonate was obtained.
[0088] (3) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:4:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and acid-hydrolyzed modified starch in a mass ratio of 1:0.2 was added dropwise, with the amount of melamine resin prepolymer being 3 times the mass of disperse dye. The mixture was reacted at 60°C for 1.5 h. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.5 times the mass of disperse dye. The mixture was reacted at 75°C for 1.5 h. After settling, ammonia water was added to neutralize the sediment. After filtration, disperse dye microcapsules were obtained.
[0089] Comparative Example 3
[0090] The difference from Example 2 is that acid-hydrolyzed modified starch is not added in the preparation method of disperse dye microcapsules.
[0091] The preparation method of disperse dye microcapsules includes the following steps:
[0092] (1) Glucose lactone, calcium carbonate (average particle size of 40 nm) and n-octanol were mixed in a mass ratio of 4:1:10 and then wet ball milled at a speed of 300 rpm for 30 min. After filtration, modified calcium carbonate was obtained.
[0093] (2) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:4:150. After stirring, the pH was adjusted to 4-5. Melamine resin prepolymer was added dropwise, with the amount of melamine resin prepolymer being 3 times the mass of disperse dye. The mixture was reacted at 60°C for 1.5 h. A mixture II of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.5 times the mass of disperse dye. The mixture was reacted at 75°C for 1.5 h. After settling, ammonia water was added to neutralize the precipitate. After filtration, disperse dye microcapsules were obtained.
[0094] Comparative Example 4
[0095] The difference from Example 2 is that conventional starch is added in the preparation method of disperse dye microcapsules.
[0096] The preparation method of disperse dye microcapsules includes the following steps:
[0097] (1) Glucose lactone, calcium carbonate (average particle size of 40 nm) and n-octanol were mixed in a mass ratio of 4:1:10 and then wet ball milled at a speed of 300 rpm for 30 min. After filtration, modified calcium carbonate was obtained.
[0098] (2) Disperse dye and modified calcium carbonate were added to water in a mass ratio of 1:4:150. After stirring, the pH was adjusted to 4-5. A mixture of melamine resin prepolymer and starch in a mass ratio of 1:0.2 was added dropwise, with the amount of melamine resin prepolymer being 3 times the mass of disperse dye. The mixture was reacted at 60°C for 1.5 h. A mixture of methyl methacrylate and ammonium persulfate in a mass ratio of 1:0.2 was added dropwise, with the amount of methyl methacrylate being 1.5 times the mass of disperse dye. The mixture was reacted at 75°C for 1.5 h. After settling, ammonia water was added to neutralize the sediment. After filtration, disperse dye microcapsules were obtained.
[0099] Performance testing
[0100] Fracture strength: GB / T3923.2-2013
[0101] Color fastness to rubbing: GB3920-2008
[0102] Light fastness: GB / T8427-2019
[0103] Table 1
[0104]
[0105]
[0106] Table 2
[0107] Color fastness to dry rubbing Color fastness to wet rubbing Light fastness Example 1 Level 5 Level 5 Level 5 Example 2 Level 4-5 Level 4-5 Level 4-5 Example 3 Level 4-5 Level 4-5 Level 4-5 Example 4 Level 4 Level 4 Level 4-5 Comparative Example 1 Level 3-4 Level 3-4 Level 3 Comparative Example 2 Level 3 Level 3 Level 3 Comparative Example 3 Level 3-4 Level 3-4 Level 3-4 Comparative Example 4 Level 3 Level 3 Level 2-3
[0108] As shown in Tables 1-2, the dyeing method of the present invention eliminates the need for desizing and washing, reducing the discharge of large amounts of wastewater and the consumption of steam, water and electricity, thus achieving energy conservation and emission reduction, reducing production costs, and producing polyester fabrics with good tensile strength, excellent dry rubbing color fastness (≥4 grade), wet rubbing color fastness (≥4 grade), and light fastness (≥4 grade), with good overall quality, huge market prospects, and significant market and economic benefits.
[0109] Comparative Example 1 shows that the addition of modified calcium carbonate facilitates better diffusion of dispersed dyes within the microcapsules and promotes better penetration of dye molecules, thereby improving color fastness. Comparative Example 2 shows that the parameters of wet ball milling are particularly important for the modification effect on the calcium carbonate surface; exceeding the specified range will cause premature bubble formation in the calcium carbonate, which is not only detrimental to microcapsule preparation but also significantly affects color fastness. Comparative Example 3 shows that acid-hydrolyzed modified starch helps improve the affinity between microcapsules and polyester fibers and also benefits the bonding strength between dyes and polyester. Comparative Example 4 shows that conventional starch has a large molecular weight and high viscosity, which is detrimental to microcapsule preparation and the dispersion of dye molecules. This results in reduced color fastness, color spots, and decreased dyeing uniformity.
[0110] The above description is merely a preferred embodiment of the present invention and is not intended to limit the present invention in any way. Any simple modifications, alterations, and equivalent transformations made to the above embodiments based on the technical essence of the present invention shall still fall within the protection scope of the present invention.
Claims
1. A dyeing method for abrasion-resistant and light-resistant polyester fabric that does not require desizing and washing, characterized in that, Includes the following steps: Step 1: Mix disperse dye microcapsules, polyacrylic acid paste, defoamer, surfactant and water evenly, adjust the pH to 5-6 to obtain dyeing paste; Step 2: Immerse the polyester fabric in the dyeing paste to obtain dyed polyester; Step 3: The dyed polyester is pre-dried, baked and set in sequence to obtain abrasion-resistant and light-resistant polyester fabric; The preparation of the disperse dye microcapsules includes: (1) Starch is added to water to make starch slurry, sulfuric acid is added for acid hydrolysis, the pH is adjusted to 3.5~5, and after post-treatment, acid hydrolyzed modified starch is obtained; (2) Glucose lactone, calcium carbonate and n-octanol in a mass ratio of 3~4:1:10 were wet ball milled at a speed of 200~300 rpm for 20~30 min and filtered to obtain modified calcium carbonate. (3) Add disperse dye and modified calcium carbonate to water and stir. Adjust the pH to 4-6. Add a mixture of amine resin prepolymer and acid-hydrolyzed modified starch (I) to carry out a preliminary reaction. Add a mixture of methyl methacrylate and ammonium persulfate (II) to carry out a second reaction. Let it stand to precipitate, add ammonia water to neutralize, and filter to obtain disperse dye microcapsules.
2. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, In step (1), the mass concentration of the starch slurry is 35-40%; the amount of sulfuric acid added is 5-8% of the starch slurry; and the acid hydrolysis is carried out at 40-45°C for 70-80 minutes.
3. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, In step (2), the particle size of the calcium carbonate is 20~100nm.
4. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, In step (3), the mass ratio of the disperse dye, modified calcium carbonate, and water is 1:4 to 6:150; the amount of melamine resin prepolymer added is 3 to 4 times the mass of the disperse dye; the mass ratio of the melamine resin prepolymer to the acid-hydrolyzed modified starch is 1:0.2 to 0.3; the amount of methyl methacrylate added is 1 to 1.5 times the mass of the disperse dye; the mass ratio of methyl methacrylate to ammonium persulfate is 1:0.1 to 0.2; the preliminary reaction is carried out at 50 to 60°C for 1 to 2 hours; and the secondary reaction is carried out at 70 to 75°C for 1 to 1.5 hours.
5. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, The ratio of the disperse dye microcapsules, polyacrylic acid slurry, defoamer, surfactant and water is 5~9g: 3~4g: 0.5~0.8g: 0.2~0.6g: 1L.
6. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, The polyacrylic slurry is an emulsion slurry obtained by crosslinking and polymerizing acrylic acid, methacrylic acid, ethyl acrylate, butyl acrylate, methyl acrylate, methyl methacrylate, acrylonitrile, and methyl methacrylate.
7. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, The defoamer is one or more of a high-carbon alcohol fatty acid ester complex, polydimethylsiloxane, and emulsified silicone oil; the surfactant is one or more of glyceryl monostearate, lauryl alcohol polyoxyethylene ether, sodium dodecylbenzenesulfonate, sodium glycocholate, and polysorbate.
8. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, The staining process involves first heating the sample to room temperature at a rate of 3-4°C / min, then maintaining the temperature at 130-140°C for 20-30 min, and finally cooling it back to room temperature at a rate of -4--2°C / min. The pH is 4-6, and the bath ratio is 1:5-10.
9. The dyeing method for abrasion-resistant and light-resistant polyester fabric without desizing and washing as described in claim 1, characterized in that, The pre-drying is carried out at a temperature of 110~120℃ with hot air for 2~3 minutes; the baking temperature is 200~210℃ and the time is 120~150 seconds.
Citation Information
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