High-crease-resistant breathable functional textile fabric, and preparation method and application thereof

Abstract

The application relates to the technical field of textile fabric finishing, in particular to a high-crease-resistance and breathable functional textile fabric and a preparation method and application thereof. The method comprises the following steps: preparing a polycarboxylic acid solution by mixing 1,2,3,4-butane tetracarboxylic acid and citric acid, partially neutralizing the carboxyl groups by using 2-amino-2-methyl-1-propanol, making the mol ratio of latent carboxyl groups to free carboxyl groups be 0.8-1.4, and then adding sodium hypophosphite monohydrate, polyethylene glycol-200 and D 90 A finishing liquid is prepared by using hydrophilic fumed silica dispersion liquid with a particle size of not more than 3 microns, polyethylene glycol-600 and non-ionic penetrant. The cotton fabric is treated by double-dipping and double-padding, and then pre-dried to a moisture regain of 5.5%-8.5%, and then baked, washed, neutralized and dried to obtain the functional fabric. The application controls the release of the reaction activity of the polycarboxylic acid, the moisture content at the end of the pre-drying, the segmented addition of PEG and the dispersion state of the silica, which is beneficial to improving the crease recovery performance and the wash-after-keeping property of the cotton fabric, maintaining the breathable pore channel of the fabric and reducing the loss of breaking strength.

Description

Technical Field

[0001] This invention relates to the field of textile finishing technology, and in particular to a highly wrinkle-resistant and breathable functional textile fabric, its preparation method, and its application. Background Technology

[0002] Cotton fabrics are composed of cellulose fibers and possess advantages such as good moisture absorption, comfortable wear, and strong skin-friendliness, making them widely used in shirts, trousers, bedding, and home textiles. However, cellulose molecules contain a large number of hydroxyl groups, which makes the fibers prone to relative slippage and hydrogen bond rearrangement under external forces, leading to wrinkles after wearing, washing, or folding. For apparel fabrics such as shirts, which require a high degree of smoothness, wrinkle-resistant finishing is an important post-treatment process to improve ease of care.

[0003] Traditional wrinkle-free or anti-wrinkle finishing often uses resin cross-linking systems containing formaldehyde or potentially releasing formaldehyde. These systems can form cross-linked structures between cellulose molecular chains, improving the fabric's wrinkle recovery performance. However, during processing and use, there may be issues such as controlling free formaldehyde, stiffening of the hand feel, decrease in strength, and stricter environmental requirements. With consumers increasingly focusing on ecological safety and wearing comfort, formaldehyde-free anti-wrinkle finishing has become an important development direction for cotton fabric finishing.

[0004] Polycarboxylic acid finishing agents are a class of systems that have attracted much attention in formaldehyde-free wrinkle-resistant finishing. Polycarboxylic acids such as 1,2,3,4-butanetetracarboxylic acid and citric acid can undergo esterification reactions with the hydroxyl groups of cellulose under catalytic and baking conditions, thereby improving the wrinkle recovery ability of fabrics. Compared with traditional formaldehyde-containing resins, polycarboxylic acid systems have advantages in formaldehyde release. However, due to the strong acidity of the reaction system and the fact that esterification crosslinking usually requires high temperatures, acid-heat damage to cotton fibers may still occur during the finishing process, manifesting as decreased breaking strength, stiffer hand feel, or changes in whiteness.

[0005] CN109137499B discloses an anti-wrinkle finishing liquid for cotton fabrics and its application. This solution uses butanetetracarboxylic acid, sodium hypophosphite, chitosan, and modified cellulose nanocrystals to improve the wrinkle resistance and strength retention of cotton fabrics through a two-dip, two-nip, pre-drying, and baking process. This solution demonstrates that the BTCA system can achieve good anti-wrinkle effects, but it mainly improves the strength after polycarboxylic acid crosslinking by reinforcing components, with insufficient attention paid to the synergistic control of the reaction initiation timing, the moisture content at the end of the fabric pre-drying, and the retention of pores between yarns. For high-density pure cotton shirt fabrics, if the finishing liquid leaves free liquid bridges between yarns or premature local esterification occurs during the pre-drying stage, it may still cause film formation at the pores, decreased air permeability, or strength loss.

[0006] CN106087391A discloses a method for preparing a wrinkle-resistant, soft, breathable, and pollution-free composite functional fabric. This method uses polycarboxylic acids, cyclodextrin, a catalyst, a multi-amino-terminated polymer, and nano-titanium dioxide as components for composite functional finishing, achieving a balance of antibacterial, UV-resistant, deodorizing, self-cleaning, and certain wrinkle-resistant properties. This method emphasizes the load-bearing capacity of functional materials and the multi-functional composite effect. The processing flow also involves padding, pre-drying, and baking, but it does not address the contradiction between "wrinkle resistance enhancement and maintaining breathability and strength" in polycarboxylic acid wrinkle finishing, nor does it propose detailed solutions for releasing reactive activity and controlling moisture content.

[0007] Therefore, in formaldehyde-free polycarboxylic acid finishing processes, avoiding the decrease in strength and air permeability caused by simply increasing the degree of crosslinking, while ensuring high wrinkle recovery after washing, remains a problem to be solved in the functional finishing of pure cotton shirt fabrics. Especially under continuous industrial two-dip and two-roll production conditions, a finishing method with measurable parameters, scalable processes, and verifiable performance is needed to concentrate the anti-wrinkle reaction at an appropriate stage and minimize adverse effects on the air permeability channels between yarns and the mechanical properties of the fibers. Summary of the Invention

[0008] The technical problem to be solved by this invention is: in formaldehyde-free polycarboxylic acid anti-wrinkle finishing, how to make pure cotton fabric achieve wash-resistant wrinkle recovery performance while reducing the blockage of air pores and loss of breaking strength.

[0009] To solve the above-mentioned technical problems, the present invention provides a method for preparing a highly wrinkle-resistant and breathable functional textile fabric, comprising the following steps: S1. Dissolve 1,2,3,4-butanetetracarboxylic acid and anhydrous citric acid in softened water to obtain a polycarboxylic acid solution; add 2-amino-2-methyl-1-propanol to the polycarboxylic acid solution to make the mol ratio of latent carboxyl groups formed by the ammonium carboxylate salt to unneutralized free carboxyl groups 0.8-1.4, and then add sodium hypophosphite monohydrate to obtain a semi-closed delayed-detonation polycarboxylic acid reactant solution.

[0010] S2. Polyethylene glycol-200 is added to the semi-closed, delayed-release polycarboxylic acid reactant solution, followed by a hydrophilic fumed silica dispersion, then polyethylene glycol-600 and a nonionic penetrant. After adjusting the volume, a finishing solution is obtained. The particle size D of the hydrophilic fumed silica in the hydrophilic fumed silica dispersion is... 90 No larger than 3μm.

[0011] S3. The cotton fabric is dipped and nibbled twice in the finishing solution, with the nibble rate controlled at 70% to 80%, and then pre-dried at 75 to 85°C until the fabric moisture regain is 5.5% to 8.5%.

[0012] S4. The pre-dried fabric is baked at 135-155℃ for 90-150s, then washed, neutralized and dried to obtain the high wrinkle-resistant and breathable functional textile fabric.

[0013] Furthermore, the finishing solution contains 70-90g of 1,2,3,4-butanetetracarboxylic acid and 15-25g of anhydrous citric acid per 1L.

[0014] Furthermore, the 2-amino-2-methyl-1-propanol is a 95% aqueous solution, and the temperature of the polycarboxylic acid solution during the addition process does not exceed 45°C.

[0015] Furthermore, the pH of the system after adding 2-amino-2-methyl-1-propanol is 3.8–4.3.

[0016] Furthermore, the finishing solution contains 40-60g of sodium hypophosphite monohydrate per 1L.

[0017] Furthermore, the finishing solution, per 1L, contains 15-22g of polyethylene glycol-200, 4.5-7.5g of hydrophilic fumed silica, and 10-15g of polyethylene glycol-600.

[0018] Furthermore, the specific surface area of ​​the hydrophilic fumed silica is 180–220 m². 2 / g.

[0019] Furthermore, the hydrophilic fumed silica dispersion is prepared by adding hydrophilic fumed silica to softened water and dispersing it at 2500-3500 r / min for 15-25 min.

[0020] Furthermore, the nonionic penetrant is an isomeric alcohol polyoxyethylene ether penetrant, and the finishing solution contains 1.5 to 2.5 g of the nonionic penetrant per 1 L.

[0021] Furthermore, the cotton fabric is a pure cotton woven grey fabric with an areal density of 100–140 g / m². 2 .

[0022] Furthermore, the immersion and rolling pressure of the two-dip and two-roll process is 0.20 to 0.30 MPa, and the speed is 20 to 40 m / min.

[0023] Furthermore, the neutralization is performed using a sodium carbonate solution of 1.5–2.5 g / L, at a bath ratio of 1:15–1:25 and a temperature of 35–45°C for 1–3 minutes, to bring the pH of the fabric to 6.2–6.8.

[0024] The present invention also provides a highly wrinkle-resistant and breathable functional textile fabric, which is prepared by the above-described preparation method.

[0025] The present invention also provides the application of the aforementioned highly wrinkle-resistant and breathable functional textile fabric in the preparation of shirts, jackets, trousers or bedding.

[0026] In this invention, latent carboxyl groups refer to carboxyl groups in the polycarboxylic acid solution that form an ammonium carboxylate salt with 2-amino-2-methyl-1-propanol; free carboxyl groups refer to carboxyl groups that retain a titratable acidic state after neutralization. The molar ratio of latent to free carboxyl groups is calculated based on the theoretical number of carboxyl groups that can be neutralized by the amino group in 2-amino-2-methyl-1-propanol and the number of remaining titratable carboxyl groups after neutralization. The total amount of titratable carboxyl groups in the polycarboxylic acid solution can be calculated based on the amount of 1,2,3,4-butanetetracarboxylic acid and anhydrous citric acid added, and verified by acid-base titration.

[0027] This invention employs a polycarboxylic acid reaction system composed of 1,2,3,4-butanetetracarboxylic acid and citric acid, and partially neutralizes the titratable carboxyl groups with 2-amino-2-methyl-1-propanol, controlling the molar ratio of latent carboxyl groups to free carboxyl groups at 0.8–1.4. This setup maintains a relatively mild reaction state of the finishing solution during the padding and pre-drying stages, while releasing carboxyl groups capable of participating in esterification during the baking stage at 135–155°C. This helps reduce the adverse effects of premature crosslinking or localized acid-heat during the pre-drying stage. Compared to comparative examples with no partial neutralization or excessively high neutralization ratios, this ratio range achieves a better balance between wrinkle recovery and strength retention.

[0028] This invention controls the moisture regain of the fabric at the end of the pre-drying process after padding to 5.5%–8.5%, and then proceeds with the baking process at this moisture regain. This process window significantly reduces free liquid bridges between yarns in the fabric, while retaining a certain amount of bound water near the fiber surface, which is beneficial for the short-range esterification crosslinking of polycarboxylic acid reactants near the fiber surface. As can be seen from the examples and comparative examples, insufficient wrinkle recovery occurs when the moisture regain is too low, while a decrease in air permeability retention occurs when the moisture regain is too high. Therefore, this window can better balance wrinkle resistance and air permeability retention.

[0029] This invention employs the following sequence: polyethylene glycol-200 is added first, followed by a hydrophilic fumed silica dispersion, and then polyethylene glycol-600 is added. The hydrophilic fumed silica is dispersed to D... 90 The particle size is no greater than 3 μm. Polyethylene glycol-200, with its lower molecular weight, more easily penetrates the near-surface layer of the fiber and participates in softening; polyethylene glycol-600, with its relatively higher molecular weight, is more beneficial for maintaining the softness and hand feel of the outer side of the finishing layer. Fine hydrophilic fumed silica, as a dispersing spacer component, helps reduce continuous film formation of the finishing layer in the pores between yarns. Comparative studies show that changing the order of PEG addition, omitting silica, or coarsely dispersing silica all decrease the air permeability retention and strength retention.

[0030] This invention employs a sodium hypophosphite monohydrate catalytic system, a two-dip, two-nip process, gentle pre-drying, temperature-controlled baking, and subsequent washing and neutralization steps. All parameters can be achieved using conventional textile finishing equipment, making it suitable for continuous production. The pH of the water extract from the finished fabric can be controlled to near neutral, and the system does not introduce formaldehyde-containing resins; testing according to GB / T 2912.1-2009 shows no detection. Based on the combined examples and comparative data, this invention, compared to conventional polycarboxylic acid finishing methods, can maintain high initial and post-wash crease recovery angles while improving air permeability retention and breaking strength retention. It is suitable for fabrics such as pure cotton shirts that require smoothness, breathability, and durability. Detailed Implementation

[0031] To make the objectives, technical solutions, and advantages of this invention clearer, the invention will be further described in detail below with reference to specific embodiments. Example 1:

[0032] The raw materials and specifications used in this embodiment are as follows: pure cotton woven shirt fabric, plain weave, with a surface density of 120g / m². 2 Warp and weft density 133×72 threads / inch, commercially available bleached semi-finished product; 2-amino-2-methyl-1-propanol, 95% aqueous solution; polyethylene glycol-200, number average molecular weight approximately 200; polyethylene glycol-600, number average molecular weight approximately 600; hydrophilic fumed silica, specific surface area approximately 200 m² 2 / g, with an average particle size of approximately 12nm.

[0033] Step 1: Add 80g of 1,2,3,4-butanetetracarboxylic acid and 20g of anhydrous citric acid to 600g of softened water. Stir at 300r / min for 15min at 40℃ until completely dissolved, resulting in a polycarboxylic acid solution with a titratable total carboxyl group of 1.68mol. Maintaining the temperature no higher than 40℃ and the stirring speed at 200r / min, add 79g of 2-amino-2-methyl-1-propanol aqueous solution dropwise over 20min. This amount is calculated to neutralize 50% of the total titratable carboxyl group moles in the system, ensuring a latent carboxyl group to free carboxyl group mole ratio of 1.0. After the addition is complete, continue stirring for 15min. The pH of the system is measured to be 4.0, yielding a semi-closed, delayed-detonation polycarboxylic acid reactant solution. Subsequently, add 50g of sodium hypophosphite monohydrate and stir for 10min until completely dissolved.

[0034] Step 2: Add 18g of polyethylene glycol-200 to the above reaction solution and stir for 10 minutes; separately, add 6g of hydrophilic fumed silica to 100g of softened water and disperse at a high speed of 3000r / min for 20 minutes to achieve a particle size D after dispersion. 90 A silica dispersion with a particle size not exceeding 3 μm was obtained; the dispersion was then added to the reaction solution and stirred for 15 min.

[0035] Step 3: Add 12g of polyethylene glycol-600 to the system and stir for 10 minutes; then add 2g of nonionic isomeric alcohol polyoxyethylene ether penetrant JFC-E, stir for 5 minutes, and bring the volume to 1L with softened water. The pH was measured again and found to be 4.0, thus obtaining the finishing solution.

[0036] Step 4: The pure cotton shirt fabric is dipped and nibbled twice in the finishing solution at 25℃, with a nibbling pressure of 0.25MPa and a speed of 30m / min, and the nibbling residue is controlled at 75%. Then it is pre-dried at 80℃ for 90s, and the moisture regain is monitored by the drying loss method. The moisture regain of the fabric is controlled to be 7.0% at the end of the pre-drying.

[0037] Step 5: Immediately after the above moisture regain condition, send the fabric into the baking process at a temperature of 145℃ for 120 seconds, so that the latent carboxyl groups are deactivated by heat and undergo esterification crosslinking with the cellulose hydroxyl groups under catalytic conditions.

[0038] Step 6: After baking, the fabric is washed with warm water at 40℃, then treated with a dilute sodium carbonate solution with a concentration of 2g / L at a bath ratio of 1:20 and 40℃ for 2 minutes to neutralize to pH 6.5, and finally dried at 80℃ to obtain a high wrinkle-resistant and breathable functional pure cotton shirt fabric. Example 2:

[0039] The substrate and raw material specifications used in this embodiment are the same as those in Embodiment 1.

[0040] Step 1: Add 70g of 1,2,3,4-butanetetracarboxylic acid and 15g of anhydrous citric acid to 600g of softened water. Stir at 300r / min for 15min at 40℃ until completely dissolved, resulting in a polycarboxylic acid solution with a titratable total carboxyl group of 1.43mol. Maintaining the temperature no higher than 40℃ and the stirring speed at 200r / min, add 59.7g of 2-amino-2-methyl-1-propanol aqueous solution dropwise over 20min to achieve a latent carboxyl group to free carboxyl group mol ratio of 0.8. After the addition is complete, continue stirring for 15min, and measure the pH of the system to be 3.8. Then add 40g of sodium hypophosphite monohydrate and stir for 10min until completely dissolved.

[0041] Step 2: Add 15g of polyethylene glycol-200 to the above reaction solution and stir for 10 minutes; separately, add 4.5g of hydrophilic fumed silica to 100g of softened water and disperse at 3000r / min for 20 minutes to achieve a particle size D after dispersion. 90 A silica dispersion with a particle size not exceeding 2.5 μm was obtained; the dispersion was added to the reaction solution and stirred for 15 min.

[0042] Step 3: Add 10g of polyethylene glycol-600 to the system and stir for 10 minutes; then add 1.5g of nonionic isomeric alcohol polyoxyethylene ether penetrant JFC-E and stir for 5 minutes. Adjust the volume to 1L with softened water and retest the pH to 3.8 to obtain the finishing solution.

[0043] Step 4: The pure cotton shirt fabric is dipped and nibbled twice in the finishing solution at 25℃ with a nipping pressure of 0.22MPa and a speed of 30m / min, and the nipping rate is controlled at 72%. Then it is pre-dried at 75℃ for 110s, and the moisture regain is monitored by the drying loss method. The moisture regain of the fabric at the end of the pre-drying is controlled at 5.5%.

[0044] Step 5: Immediately after the fabric has regained its moisture content, put it into the oven at 135°C for 150 seconds.

[0045] Step 6: After baking, the fabric is washed with warm water at 40℃, then treated with a dilute sodium carbonate solution with a concentration of 2g / L at a bath ratio of 1:20 and 40℃ for 2 minutes to neutralize to pH 6.4, and finally dried at 80℃ to obtain a high wrinkle-resistant and breathable functional pure cotton shirt fabric. Example 3:

[0046] The substrate and raw material specifications used in this embodiment are the same as those in Embodiment 1.

[0047] Step 1: Add 90g of 1,2,3,4-butanetetracarboxylic acid and 25g of anhydrous citric acid to 600g of softened water. Stir at 300r / min for 15min at 40℃ until completely dissolved, resulting in a polycarboxylic acid solution with a titratable total carboxyl group of 1.93mol. Maintaining the temperature no higher than 40℃ and the stirring speed at 200r / min, add 105.6g of 2-amino-2-methyl-1-propanol aqueous solution dropwise over 25min to achieve a latent carboxyl group to free carboxyl group mol ratio of 1.4. After the addition is complete, continue stirring for 15min, and the pH of the system is measured to be 4.2. Then add 60g of sodium hypophosphite monohydrate and stir for 10min until completely dissolved.

[0048] Step 2: Add 22g of polyethylene glycol-200 to the above reaction solution and stir for 10min; separately, add 7.5g of hydrophilic fumed silica to 100g of softened water and disperse at a high speed of 3200r / min for 25min to achieve a particle size D after dispersion. 90 A silica dispersion with a particle size not exceeding 3 μm was obtained; the dispersion was then added to the reaction solution and stirred for 15 min.

[0049] Step 3: Add 15g of polyethylene glycol-600 to the system and stir for 10 minutes; then add 2.5g of nonionic isomeric alcohol polyoxyethylene ether penetrant JFC-E and stir for 5 minutes. Adjust the volume to 1L with softened water and retest the pH to 4.2 to obtain the finishing solution.

[0050] Step 4: The pure cotton shirt fabric is dipped and nibbled twice in the finishing solution at 25℃, with a nibbling pressure of 0.28MPa and a speed of 28m / min, and the nibbling residue is controlled at 80%; then it is pre-dried at 85℃ for 80s, and the moisture regain is monitored by the drying loss method, and the moisture regain of the fabric at the end of the pre-drying is controlled at 8.5%.

[0051] Step 5: Immediately after the fabric has regained the moisture content mentioned above, put it into the oven at a temperature of 155°C for 90 seconds.

[0052] Step 6: After baking, the fabric is washed with warm water at 40℃, then treated with a dilute sodium carbonate solution with a concentration of 2g / L at a bath ratio of 1:20 and 40℃ for 2 minutes to neutralize to pH 6.3, and finally dried at 80℃ to obtain a high wrinkle-resistant and breathable functional pure cotton shirt fabric. Example 4:

[0053] The substrate and raw material specifications used in this embodiment are the same as those in Embodiment 1.

[0054] Step 1: Add 80g of 1,2,3,4-butanetetracarboxylic acid and 18g of anhydrous citric acid to 600g of softened water. Stir at 300r / min for 15min at 40℃ until completely dissolved, resulting in a polycarboxylic acid solution with a titratable total carboxyl group content of 1.65mol. Maintaining the temperature no higher than 40℃ and the stirring speed at 200r / min, add 80.9g of 2-amino-2-methyl-1-propanol aqueous solution dropwise over 22min to achieve a latent carboxyl group to free carboxyl group molar ratio of 1.1. After the addition is complete, continue stirring for 15min, and measure the pH of the system to be 4.1. Then add 55g of sodium hypophosphite monohydrate and stir for 10min until completely dissolved.

[0055] Step 2: Add 20g of polyethylene glycol-200 to the above reaction solution and stir for 10min; separately, add 6g of hydrophilic fumed silica to 100g of softened water and disperse at 3000r / min for 20min to achieve a particle size D after dispersion. 90 A silica dispersion with a particle size not exceeding 2.5 μm was obtained; the dispersion was added to the reaction solution and stirred for 15 min.

[0056] Step 3: Add 14g of polyethylene glycol-600 to the system and stir for 10 minutes; then add 2g of nonionic isomeric alcohol polyoxyethylene ether penetrant JFC-E, stir for 5 minutes, and bring the volume to 1L with softened water. The pH was measured again and found to be 4.1, thus obtaining the finishing solution.

[0057] Step 4: The pure cotton shirt fabric is dipped and nibbled twice in the finishing solution at 25℃, with a nibbling pressure of 0.25MPa and a speed of 30m / min, and the nibbling residue is controlled at 75%; then it is pre-dried at 82℃ for 85s, and the moisture regain is monitored by the drying loss method, and the moisture regain of the fabric at the end of the pre-drying is controlled at 6.5%.

[0058] Step 5: Immediately after the fabric has regained its moisture content, put it into the oven at 150°C for 100 seconds.

[0059] Step 6: After baking, the fabric is washed with warm water at 40℃, then treated with a dilute sodium carbonate solution with a concentration of 2g / L at a bath ratio of 1:20 and 40℃ for 2 minutes to neutralize to pH 6.5, and finally dried at 80℃ to obtain a high wrinkle-resistant and breathable functional pure cotton shirt fabric.

[0060] Comparative Example 1: The difference from Example 1 is that: in step one, 2-amino-2-methyl-1-propanol aqueous solution is not added, and it is replaced by an equal amount of 79g softened water so that the mol ratio of latent carboxyl groups to free carboxyl groups is 0. The other conditions are the same as in Example 1.

[0061] Comparative Example 2: The difference from Example 1 is that the amount of 2-amino-2-methyl-1-propanol aqueous solution added in step one is adjusted to 105g, so that the mol ratio of latent carboxyl groups to free carboxyl groups is 2.0, and the other conditions are the same as in Example 1.

[0062] Comparative Example 3: The difference from Example 1 is that the moisture regain of the fabric at the end of the pre-drying process in step four is controlled at 3.0%, while the other conditions are the same as in Example 1.

[0063] Comparative Example 4: The difference from Example 1 is that the moisture regain of the fabric at the end of the pre-drying process in step four is controlled at 12.0%, while the other conditions are the same as in Example 1.

[0064] Comparative Example 5: The difference from Example 1 is that the baking temperature in step five is 125°C and the time is 120 seconds, while the other conditions are the same as in Example 1.

[0065] Comparative Example 6: The difference from Example 1 is that the baking temperature in step five is 165°C and the time is 120 seconds, while the other conditions are the same as in Example 1.

[0066] Comparative Example 7: The difference from Example 1 is that in step two, 18g of polyethylene glycol-200 and 12g of polyethylene glycol-600 were added to the reaction solution at the same time, and then a hydrophilic fumed silica dispersion was added. The other conditions were the same as in Example 1.

[0067] Comparative Example 8: The difference from Example 1 is that 6g of hydrophilic fumed silica is not added in step two, and 106g of softened water is used to replace the silica dispersion. The other conditions are the same as in Example 1.

[0068] Comparative Example 9: The difference from Example 1 is that in step two, the dispersion conditions for the hydrophilic fumed silica are changed to 1000 r / min for 5 min, so that the dispersion D 90 The thickness is 7.5–8.5 μm, and the other conditions are the same as in Example 1.

[0069] Performance testing Silica dispersion particle size D 90 Take 1 mL of the silica dispersions prepared in each example and comparative example, before adding them to the reaction solution, dilute with softened water to a mass fraction of 0.05%, and determine the particle size distribution using a laser particle size analyzer according to GB / T19077-2024 "Particle Size Analysis - Laser Diffraction Method". Each sample was measured in triplicate, and the particle size distribution (D) was recorded. 90 Values ​​are in μm; samples without added silica are recorded as "Not Applicable".

[0070] Pre-drying endpoint fabric moisture regain: Take approximately 5g of fabric sample that has been pre-dried but not yet fully baked, immediately place it in a sealed weighing bottle, and dry it to constant weight at 105±2℃ according to GB / T 9995-1997 "Determination of Moisture Content and Moisture Regain of Textile Materials - Oven Drying Method". Calculate the moisture regain using the formula: Moisture regain = (Pre-dried mass − Constant dried mass) / Constant dried mass × 100%. Take 3 samples from different locations in each group of samples, and take the average value. The unit is %.

[0071] Weight gain rate of finishing agent: The same batch of pure cotton grey fabric was cut into 200mm×200mm samples and conditioned for 24 hours at 20±2℃ and 65±4% relative humidity according to GB / T 6529-2008. The dry weight m0 before finishing was measured. After finishing, washing, neutralization, and drying, the fabric was conditioned again for 24 hours, and the dry weight m1 after finishing was measured. The weight gain rate was calculated as (m1−m0) / m0×100%. Five samples were used in each group, and the average value was taken. The unit is %.

[0072] pH of the fabric aqueous extract: Cut the finished fabric into small pieces of approximately 5mm × 5mm. Add 2.00g of sample to 100mL of grade III water according to GB / T 7573-2009 "Determination of pH of Aqueous Extracts from Textiles". Shake at room temperature for 2 hours. Measure the pH of the extract using a pH meter calibrated with pH 4.00, 6.86, and 9.18 buffer solutions. Perform three replicates per group, and take the average result.

[0073] Free and hydrolyzed formaldehyde content: Take 1.00g of the finished fabric and perform water extraction and acetylacetone colorimetric reaction according to GB / T 2912.1-2009 "Textiles - Determination of formaldehyde - Part 1: Free and hydrolyzed formaldehyde (water extraction method)". Measure the absorbance at 412nm using a UV-Vis spectrophotometer. Each group is divided into three replicates. A concentration below 20mg / kg is recorded as undetectable.

[0074] Initial wrinkle recovery angle: Tested according to GB / T 3819-1997 "Textiles - Determination of Crease Recovery of Fabrics - Method of Recovery Angle". After conditioning each sample in the standard atmosphere of GB / T 6529-2008 for 24 hours, five 40mm×15mm samples were cut along the warp and five along the weft directions. A 10N load was applied for 5 minutes, and after unloading, the samples recovered for 5 minutes. The warp and weft wrinkle recovery angles were measured, and the sum of the warp average and the weft average was taken as the total wrinkle recovery angle, in degrees.

[0075] Wrinkle recovery angle after 10 household washes: According to GB / T 8629-2017 "Domestic washing and drying procedures for testing textiles", the samples were washed and dried 10 times using a type A standard washing machine, 4N program, standard detergent, and hanging drying method. After washing, the samples were conditioned for 24 hours according to GB / T 6529-2008, and then the total wrinkle recovery angle was measured according to GB / T 3819-1997. The sum of the average values ​​of 5 samples in the warp and weft directions was taken, and the unit was °.

[0076] Air permeability and air permeability retention rate: tested according to GB / T 5453-1997 "Textiles - Determination of Air Permeability of Fabrics". After conditioning the samples for 24 hours, an air permeability tester was used, with a test area of ​​20 cm². 2 The pressure difference of the fabric was 100 Pa. Ten measurements were taken at different locations for each group, and the average air permeability was recorded in mm / s. Air permeability retention rate = (Air permeability of finished sample / Air permeability of unfinished fabric in the same batch) × 100%, in %.

[0077] Tensile strength retention rate: Tested according to GB / T 3923.1-2013 "Textiles - Tensile Properties of Fabrics - Part 1: Determination of Tensile Strength and Elongation at Break (Strip Method)". After conditioning the samples for 24 hours, five samples with an effective width of 50±0.5mm were cut along the warp direction, with a spacing of 200mm. The tensile speed was 100mm / min, and the maximum tensile strength was recorded. Tensile strength retention rate = warp tensile strength of finished sample / warp tensile strength of unfinished fabric in the same batch × 100%, in units of 100%.

[0078] Table 1 Performance test results of the examples and comparative examples

[0079] Data Analysis: As shown in Table 1, after finishing, Examples 1-4 all increased the initial wrinkle recovery angle of the pure cotton fabric from 139.4° to 248.7-267.2°, and maintained it at 225.1-242.7° after 10 household washes. At the same time, the air permeability retention rate was 86.5%-91.9%, and the breaking strength retention rate was 78.4%-84.6%. This indicates that under the conditions of a latent carboxyl group / free carboxyl group mol ratio of 0.8-1.4, a pre-drying endpoint moisture regain of 5.5%-8.5%, and a baking temperature of 135-155℃, a good balance between wrinkle resistance, air permeability, and strength retention can be achieved.

[0080] Compared to Example 1, Comparative Example 1 did not form latent carboxyl groups. Although the initial wrinkle recovery angle still reached 246.1°, the air permeability retention rate decreased to 77.3% and the tensile strength retention rate decreased to 66.8%, indicating that a purely free carboxyl system may lead to premature or excessive concentration of the finishing reaction. Comparative Example 2 had an excessively high proportion of latent carboxyl groups, and the initial and post-wash wrinkle recovery angles decreased to 232.8° and 205.9°, respectively, indicating that a latent carboxyl group proportion exceeding a suitable range is not conducive to effective crosslinking retention. Comparative Examples 3 and 5 had significantly reduced wrinkle recovery angles and post-wash retention rates due to excessively low moisture regain or excessively low baking temperatures, respectively. Comparative Example 4, due to its excessively high moisture regain, had an air permeability retention rate of only 72.0%, possibly related to the incomplete breaking of free liquid bridges between yarns. Comparative Example 6, while maintaining a high initial wrinkle recovery angle at 165°C, saw its breaking strength retention rate drop to 63.7%, indicating that excessively high baking temperatures exacerbate fabric damage. Comparative Example 7, by changing the order of PEG addition, Comparative Example 8, by removing hydrophilic fumed silica, and Comparative Example 9, by coarsely dispersing silica, all showed lower air permeability and strength retention rates than Example 1, indicating that segmented PEG addition and fine silica dispersion are beneficial in maintaining open pores while reducing strength loss. Overall, the present invention provides a more balanced effect in terms of washability, wrinkle resistance, air permeability retention, and breaking strength retention compared to the comparative examples.

[0081] Those skilled in the art should understand that the discussion of any of the above embodiments is merely exemplary and is not intended to imply that the scope of the invention is limited to these examples; within the framework of the invention, the technical features of the above embodiments or different embodiments can also be combined, and there are many other variations of the different aspects of the invention as described above, which are not provided in detail for the sake of brevity.

Claims

1. A method for preparing a highly wrinkle-resistant and breathable functional textile fabric, characterized in that, Includes the following steps: (1) Dissolve 1,2,3,4-butanetetracarboxylic acid and anhydrous citric acid in softened water to obtain a polycarboxylic acid solution; add 2-amino-2-methyl-1-propanol to the polycarboxylic acid solution so that the mol ratio of latent carboxyl groups formed by the ammonium carboxylate salt to unneutralized free carboxyl groups is 0.8 to 1.4, and then add sodium hypophosphite monohydrate to obtain a semi-closed delayed-decongestion polycarboxylic acid reactant solution; (2) Polyethylene glycol-200 was added to the semi-closed, delayed-deblocking polycarboxylic acid reactant solution, followed by the addition of a hydrophilic fumed silica dispersion, then polyethylene glycol-600 and a nonionic penetrant, and the solution was brought to a final volume to obtain a finishing solution; the particle size D of the hydrophilic fumed silica in the hydrophilic fumed silica dispersion was... 90 No larger than 3μm; (3) The cotton fabric is dipped and nibbled twice in the finishing solution, with the nibble rate controlled at 70% to 80%, and then pre-dried at 75 to 85°C until the fabric moisture regain is 5.5% to 8.5%; (4) The pre-dried fabric is baked at 135-155℃ for 90-150s, then washed, neutralized and dried to obtain the high wrinkle-resistant and breathable functional textile fabric.

2. The preparation method according to claim 1, characterized in that, The finishing solution, per 1L, contains 70–90g of 1,2,3,4-butanetetracarboxylic acid, 15–25g of anhydrous citric acid, 40–60g of sodium hypophosphite monohydrate, 15–22g of polyethylene glycol-200, 4.5–7.5g of hydrophilic fumed silica, 10–15g of polyethylene glycol-600, and 1.5–2.5g of the nonionic penetrant.

3. The preparation method according to claim 1, characterized in that, The 2-amino-2-methyl-1-propanol is a 95% aqueous solution. During the addition process, the temperature of the polycarboxylic acid solution does not exceed 45°C, and the pH of the system after adding 2-amino-2-methyl-1-propanol is 3.8 to 4.

3.

4. The preparation method according to claim 1, characterized in that, The specific surface area of ​​the hydrophilic fumed silica is 180–220 m². 2 / g.

5. The preparation method according to claim 1, characterized in that, The hydrophilic fumed silica dispersion is prepared by adding hydrophilic fumed silica to softened water and dispersing it at 2500-3500 r / min for 15-25 min.

6. The preparation method according to claim 1, characterized in that, The cotton fabric is a pure cotton woven grey fabric with a surface density of 100–140 g / m². 2 .

7. The preparation method according to claim 1, characterized in that, The immersion and rolling pressure of the two dips and two rolls is 0.20-0.30 MPa, and the speed is 20-40 m / min.

8. The preparation method according to claim 1, characterized in that, The neutralization process uses a sodium carbonate solution of 1.5–2.5 g / L, treated at a bath ratio of 1:15–1:25 and a temperature of 35–45°C for 1–3 minutes, to bring the fabric pH to 6.2–6.

8.

9. A highly wrinkle-resistant and breathable functional textile fabric, characterized in that, It is prepared by the preparation method according to any one of claims 1 to 8.

10. The use of the highly wrinkle-resistant and breathable functional textile fabric of claim 9 in the preparation of shirts, jackets, trousers or bedding.

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