Preparation method of shrink-proof anti-wrinkle all-cotton textile fabric

Abstract

The invention relates to the technical field of fabric research and development, and provides a preparation method of a shrink-proof anti-wrinkle all-cotton textile fabric. Comprising the following steps: selecting long stapled cotton fibers improved by gene editing, carrying out ultrasonic-assisted enzymolysis pretreatment on all-cotton fibers, preparing a treating fluid containing a novel bifunctional crosslinking agent, dipping the pretreated fabric in the treating fluid, and carrying out ultrasonic-assisted enzymolysis treatment on all-cotton fibers; a cross-linking agent is promoted to uniformly permeate into fibers by utilizing a pulsed electric field assisted permeation technology, the surfaces of the fibers are activated through low-temperature plasmas, and after-finishing treatment is performed by adopting a segmented temperature control heat setting process. The preparation method of the high-performance shrink-proof anti-wrinkle all-cotton textile fabric integrates gene editing material innovation, advanced enzymolysis pretreatment, intelligent cross-linking agent design, multi-physical-field auxiliary permeation and low-temperature plasma activation, segmented temperature control heat setting and green after-treatment, the anti-wrinkle recovery rate of the fabric is increased, the shrinkage rate is reduced, and the fabric quality is improved. The air permeability, the softness and the self-repairing capability are improved.

Description

Technical Field

[0001] The invention relates to the technical field of fabric research and development, and in particular to a method for preparing shrinkage-resistant and wrinkle-resistant pure cotton textile fabric. Background Art

[0002] 100% cotton textiles are widely used in clothing, home textiles, and other fields due to their excellent comfort, breathability, and natural environmental properties. However, traditional 100% cotton fabrics are prone to wrinkling and shrinkage, which seriously affects their performance and consumer experience. In particular, during washing and wearing, the internal stress release of cotton fibers causes irreversible wrinkling and dimensional changes in the fabric, reducing the product's aesthetics and durability.

[0003] To improve the wrinkle resistance of all-cotton fabrics, traditional methods often use chemical crosslinking agents, such as formaldehyde or formaldehyde-free crosslinking agents, to crosslink the fibers. However, these methods can lead to problems such as residual crosslinking agents, stiffness in the fabric, decreased breathability, and environmental pollution. Furthermore, traditional crosslinking agents are often irreversible and lack the fabric's self-repairing properties, limiting the fabric's lifespan.

[0004] In fiber pretreatment, enzymatic hydrolysis technology is widely used for fiber surface modification due to its mild and environmentally friendly properties. However, the enzymatic hydrolysis process is typically time-consuming and has limited enzyme penetration, making it difficult to form an ideal micropore structure, which in turn affects the subsequent bonding of crosslinkers. Furthermore, traditional heat setting processes often rely on a single high-temperature treatment, which can easily cause stress concentration within the fiber, leading to fiber embrittlement, yellowing, and decreased mechanical properties.

[0005] In recent years, the rapid development of gene editing technology has provided new insights into improving the performance of textile raw materials. By regulating genes involved in cellulose synthesis, the crystallinity and heat resistance of cotton fibers can be effectively enhanced, laying the foundation for the production of high-performance textiles. Furthermore, the design of dynamic reversible crosslinkers, which impart self-healing capabilities to fabrics, has become an important approach for improving textile functionality.

[0006] In addition, the introduction of advanced physical auxiliary technologies such as ultrasound-assisted enzymatic hydrolysis, pulsed electric field-assisted penetration and low-temperature plasma activation has provided an effective means to improve the efficiency of fiber surface modification and the uniformity of cross-linker penetration. However, the systematic application of related technologies in all-cotton shrinkage-resistant and wrinkle-resistant fabrics is still immature and urgently needs further research and improvement.

[0007] In summary, existing technologies still struggle to achieve the desired combination of high wrinkle recovery, low shrinkage, good breathability, and environmentally friendly self-repair properties for all-cotton fabrics. Furthermore, the processing is complex and inefficient, making it difficult to meet the demands of the modern high-end textile market. Therefore, developing a method for preparing highly efficient, shrink-resistant, and wrinkle-resistant all-cotton fabrics based on gene-edited modified fibers, combined with enzymatic pretreatment, dynamic crosslinking agents, and multi-physics field-assisted technologies, is of great technical significance and application value. Summary of the Invention

[0008] In order to overcome the defects of the prior art, the object of the present invention is to provide a method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric.

[0009] To achieve the above object, the technical solution of the present invention is implemented as follows: a method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric, comprising the following steps:

[0010] (1) Select long-staple cotton fibers that have been genetically modified to have higher fiber strength and uniform fiber diameter;

[0011] (2) Ultrasonic-assisted enzymatic pretreatment of cotton fibers was performed. By controlling the ultrasonic power and enzyme concentration, a nano-scale microporous structure was formed on the fiber surface to enhance the binding force of the subsequent cross-linking agent;

[0012] (3) preparing a treatment solution containing a novel bifunctional crosslinker, which contains a reversible crosslinking group and a nanoscale catalyst carrier. The crosslinker achieves inter-fiber crosslinking through dynamic covalent bonds and can partially break under specific conditions to release stress;

[0013] (4) Immersing the pretreated fabric in the treatment solution, using pulsed electric field assisted penetration technology to promote the crosslinking agent to evenly penetrate the fiber interior, with an immersion time of 3 to 15 minutes;

[0014] (5) Treating the fiber surface with low-temperature plasma activation further enhances the bonding stability between the crosslinker and the fiber and the anti-wrinkle performance of the fabric;

[0015] (6) Using a segmented temperature-controlled heat setting process, multi-stage heating treatment is performed in the range of 90°C to 140°C to control the time and temperature gradient, optimize the internal stress distribution of the fiber, and achieve excellent anti-shrinkage and anti-wrinkle effects;

[0016] (7) Perform post-finishing treatment, which includes supercritical CO2 extraction and cleaning to remove unreacted residues and improve the soft feel and environmental performance of the fabric.

[0017] Preferably, the gene-edited long-staple cotton fiber regulates cellulose synthesis-related genes through CRISPR-Cas9 technology to improve the fiber crystallinity and heat resistance.

[0018] Preferably, in the ultrasound-assisted enzymatic hydrolysis pretreatment step, the ultrasonic frequency is controlled at 20-40 kHz, the enzyme is a cellulase complex enzyme preparation, and the pretreatment time is 10-30 minutes.

[0019] Preferably, the novel bifunctional crosslinker is a polymer network structure containing a dynamic imine bond and a nano zinc oxide catalyst, which has both efficient crosslinking ability and self-healing properties.

[0020] Preferably, the pulsed electric field assisted penetration technology uses an electric field strength of 0.5-2 kV / cm, a pulse width of 100-500 μs, and a frequency of 10-100 Hz to improve the crosslinker penetration efficiency and uniformity.

[0021] Preferably, the low-temperature plasma activation treatment uses oxygen or argon plasma, with a treatment time of 30 seconds to 3 minutes and a power of 50-150 W.

[0022] Preferably, the segmented temperature-controlled heat setting process realizes multi-stage temperature curve control through an intelligent temperature control system, with the first stage being 90-110°C and the second stage being 120-140°C, each maintained for 1-3 minutes.

[0023] Preferably, the supercritical CO2 extraction conditions are a temperature of 35-45°C, a pressure of 10-15 MPa, and an extraction time of 20-40 minutes.

[0024] Preferably, the prepared cotton fabric has an anti-wrinkle performance of a wrinkle recovery rate of ≥90%, a shrinkage rate of ≤2%, and has excellent air permeability and durability.

[0025] Preferably, the fabric also has a certain self-repair function. After microcracks are generated under stress, the fabric structure is repaired by breaking and reorganizing dynamic cross-linking bonds, thereby extending the service life of the fabric.

[0026] The beneficial effects of the present invention are embodied in:

[0027] By utilizing long-staple cotton fibers modified through CRISPR-Cas9 gene editing, this method significantly enhances the fiber's crystallinity and heat resistance, providing a solid physical foundation for subsequent enzymatic pretreatment and crosslinking reactions. Ultrasonic-assisted enzymatic pretreatment effectively forms a uniform nanoscale microporous structure on the fiber surface within a short period of time (15 minutes), significantly enhancing the penetration depth and binding strength of the crosslinker. This method offers superior treatment efficiency and effectiveness compared to traditional enzymatic pretreatment alone.

[0028] The formulated bifunctional crosslinker, containing a dynamic imine bond and a nano-zinc oxide catalyst, not only achieves a self-repairing function that is difficult to achieve with traditional crosslinkers, but also promotes the uniformity and stability of the crosslinking reaction through the nano-catalyst, effectively improving the wrinkle recovery rate and durability of the fabric. Pulsed electric field-assisted penetration technology promotes the uniform distribution and deep penetration of the crosslinker, further enhancing the crosslinking effect and the overall performance of the fabric.

[0029] The low-temperature plasma activation step activates the fiber surface, improving the bond stability between the crosslinker and the fiber, and optimizing the fabric's wrinkle resistance and feel. The segmented temperature-controlled heat setting process scientifically controls the temperature gradient to rationally release internal fiber stress, avoiding the fiber embrittlement and localized yellowing associated with traditional single-stage high-temperature heat setting. This significantly improves the fabric's shrinkage resistance and appearance.

[0030] The finishing process utilizes supercritical CO2 extraction technology, effectively removing unreacted residues and enhancing the fabric's softness and environmental performance, in line with the development trend of green textiles. The overall process balances functionality with environmental considerations. The resulting all-cotton textile boasts a wrinkle recovery rate of up to 92%, extremely low shrinkage (1.5%), and excellent breathability (450 L / m² / s). It also exhibits exceptional self-healing properties (microcracks heal by 80% within 30 minutes at 80°C), significantly outperforming traditional processes and unmodified materials.

[0031] By comparing the experimental data, it can be seen that the gene-edited fibers, ultrasonic-assisted enzymatic hydrolysis, dynamic crosslinker formula and multi-physical field collaborative processing technology adopted in the present invention have formed a comprehensive advantage of synergistic efficiency, overcoming the bottleneck problems in the existing technology such as the difficulty in balancing anti-wrinkle and anti-shrinkage properties, the stiffness and lack of comfort of the fabric, and the lack of self-repair ability, greatly improving the functionality and usage experience of the cotton fabric.

[0032] In summary, the present invention provides a method for preparing high-performance, shrinkage-resistant, wrinkle-resistant cotton textile fabrics that integrates innovative gene-editing materials, advanced enzymatic pretreatment, intelligent crosslinker design, multi-physics field-assisted penetration and low-temperature plasma activation, segmented temperature-controlled heat setting, and environmentally friendly finishing. This method not only significantly improves the fabric's wrinkle recovery rate, reduces shrinkage, and improves breathability and softness, but also imparts excellent self-repair capabilities and extends its service life. This method meets the dual functional and environmental demands of high-end textiles and has broad market application prospects and promotional value. BRIEF DESCRIPTION OF THE DRAWINGS

[0033] In the attached figure:

[0034] Figure 1 Schematic diagram of the production method of the present invention. DETAILED DESCRIPTION

[0035] The present invention will be further described in detail below with reference to the accompanying drawings and embodiments. Obviously, the embodiments described are only some embodiments of the invention, not all embodiments. In the absence of conflict, the embodiments and features in the embodiments of this application can be combined with each other. Based on the embodiments of the invention, all other embodiments obtained by ordinary technicians in this field without making creative efforts are within the scope of protection of the invention.

[0036] In addition, the technical solutions between the various embodiments can be combined with each other, but they must be based on the fact that ordinary technicians in this field can implement them. When the combination of technical solutions is mutually contradictory or cannot be implemented, it should be deemed that such a combination of technical solutions does not exist and is not within the scope of protection required by the invention.

[0037] Please refer to the instruction manual Figure 1 The present invention provides a method for preparing shrinkage-resistant and wrinkle-resistant cotton textile fabrics:

[0038] Example 1

[0039] Step 1: Raw Material Preparation: Select long-staple cotton fibers modified through CRISPR-Cas9 gene editing. This modified cotton fiber modulates genes related to cellulose synthesis to increase the fiber's crystallinity and heat resistance, enhancing the effectiveness of subsequent processing.

[0040] Step 2: Ultrasonic-Assisted Enzymatic Pretreatment: Long-staple cotton fibers were placed in an enzymatic solution containing a cellulase complex at a concentration of 150 U / g for 15 minutes. The ultrasonic frequency was set at 25 kHz and the ultrasonic power was 50 W, and the ultrasonic-assisted enzymatic pretreatment lasted for 15 minutes. This treatment formed a nanoporous structure on the fiber surface, enhancing the binding strength of the subsequent crosslinker.

[0041] Step 3: Prepare a bifunctional crosslinker treatment solution to prepare a polymer network crosslinker containing dynamic imine bonds and nano-zinc oxide catalysts. This crosslinker has reversible crosslinking groups that can partially break under specific conditions (such as pH changes), releasing stress and achieving self-repair.

[0042] Step 4: Pulsed Electric Field-Assisted Penetration: The pretreated fibers were immersed in the crosslinker solution and a pulsed electric field was applied to promote uniform crosslinker penetration. The electric field intensity was set to 1.0 kV / cm, the pulse width to 200 μs, the frequency to 50 Hz, and the immersion time to 10 minutes.

[0043] Step 5: Low-temperature plasma activation: Argon plasma is used to activate the fiber surface at a power of 100 W for 1 minute. This step enhances the bonding stability between the crosslinker and the fiber and improves the wrinkle resistance of the fabric.

[0044] Step 6: Segmented Temperature Control Heat Setting: An intelligent temperature control system is used to increase the temperature in multiple stages: the first stage is maintained at 100°C for 2 minutes, and the second stage is maintained at 130°C for 2 minutes. By controlling the temperature gradient, the internal stress distribution of the fiber is optimized, achieving excellent wrinkle and shrinkage resistance.

[0045] Step 7: Finishing - Supercritical CO2 Extraction: The fabric is extracted in supercritical CO2 at 40°C, 12 MPa, and 30 minutes. This step removes unreacted residues, improving the fabric's softness and environmental performance.

[0046] Performance testing: The fabric has a wrinkle recovery rate of 92%, a shrinkage rate of 1.5%, and a breathability of 450 L / m² / s. Its self-healing properties show that microcracks (<10 μm) recover 80% in 30 minutes at 80°C.

[0047] Example 2

[0048] Step 1: Prepare the ingredients

[0049] We use long-staple cotton fibers modified through CRISPR-Cas9 gene editing. This modified cotton fiber modulates genes related to cellulose synthesis to increase fiber crystallinity and heat resistance, enhancing the effectiveness of subsequent treatments.

[0050] Step 2: Ultrasonic-assisted enzymatic pretreatment

[0051] Long-staple cotton fibers were pretreated with a cellulase complex at a concentration of 150 U / g for 15 minutes. Ultrasonic frequency was set at 25 kHz and power at 40 W, and the ultrasound-assisted enzymatic hydrolysis process lasted for 15 minutes. This treatment formed a nanoscale microporous structure on the fiber surface, enhancing the binding strength of the subsequent crosslinking agent.

[0052] Step 3: Prepare bifunctional crosslinker treatment solution

[0053] A polymer network crosslinker containing dynamic imine bonds and nano-zinc oxide catalysts was prepared. The crosslinker has reversible crosslinking groups that can partially break under specific conditions (such as pH changes), releasing stress and achieving self-repair.

[0054] Step 4: Pulsed electric field assisted penetration

[0055] The pretreated fibers were immersed in a crosslinker solution and a pulsed electric field was applied to promote uniform crosslinker penetration. The electric field intensity was set to 1.0 kV / cm, the pulse width was 200 μs, the frequency was 50 Hz, and the immersion time was 10 minutes.

[0056] Step 5: Low-temperature plasma activation

[0057] Argon plasma was used for fiber surface activation at a power of 100 W for 1 minute. This step enhanced the bonding stability between the crosslinker and the fiber and improved the wrinkle resistance of the fabric.

[0058] Step 6: Segmented temperature control and heat setting

[0059] The intelligent temperature control system uses a multi-stage heating process: the first stage is maintained at 90°C for 3 minutes, and the second stage is maintained at 120°C for 3 minutes. By controlling the temperature gradient, the internal stress distribution of the fiber is optimized, achieving excellent wrinkle and shrinkage resistance.

[0060] Step 7: Finishing - Supercritical CO2 Extraction

[0061] The fabric is extracted in supercritical carbon dioxide at 40°C, 12 MPa, and 30 minutes. This step removes unreacted residues, improving the fabric's softness and environmental performance.

[0062] Performance test: Wrinkle recovery rate: 89%, shrinkage rate: 1.8%, air permeability: 420 L / m² / s.

[0063] Example 3

[0064] Adjust the crosslinker type:

[0065] Step 3: The nanocatalyst in the cross-linker is replaced with titanium dioxide (3 wt%).

[0066] Performance test: Wrinkle recovery rate: 90%, catalytic activity slightly reduced, self-repair time extended to 50 minutes.

[0067] Comparative Example 1 (no gene editing)

[0068] Step 1: Use ordinary long-staple cotton, not genetically edited (crystallinity 65%, strength 5.0 cN / dtex). Other steps are the same as in Example 1.

[0069] Performance test: Wrinkle recovery rate: 78%, shrinkage rate: 3.5%, the fiber tends to become brittle after heat setting.

[0070] Comparative Example 2 (without ultrasound-assisted enzymatic hydrolysis)

[0071] Step 2: Enzymatic treatment only (without ultrasound) and the time is extended to 60 minutes.

[0072] Performance test: The fiber surface micropores are uneven, and the crosslinker penetration depth is only the surface layer. Wrinkle recovery rate: 82%, shrinkage rate: 2.8%.

[0073] Comparative Example 3 (traditional crosslinking agent)

[0074] Step 3: Use traditional DMDHEU cross-linker (no dynamic bond).

[0075] Performance testing: Wrinkle recovery rate: 85%, shrinkage rate: 2.0%. Fabric stiffness increased, breathability decreased to 300 L / m² / s, and no self-repair function was found.

[0076] Comparative Example 4 (single-stage heat setting)

[0077] Step 6: Directly treat at 140°C for 4 minutes.

[0078] Performance test: Stress concentration inside the fiber, localized yellowing. Wrinkle recovery rate: 83%, shrinkage rate: 2.5%.

[0079] Data comparison table

[0080] Test items Example 1 Example 2 Comparative Example 1 Comparative Example 3 Wrinkle recovery rate (%) 92 89 78 85 Shrinkage rate (%) 1.5 1.8 3.5 2.0 Air permeability (L / m² / s) 450 420 380 300 Self-repair capability excellent good none none

[0081] The above description is only a preferred embodiment of the present invention and is not intended to limit the present invention. Any modifications, equivalent replacements, improvements, etc. made within the spirit and principles of the present invention should be included in the scope of protection of the present invention.

[0082] It will be apparent to those skilled in the art that the present invention is not limited to the details of the exemplary embodiments described above and that the invention can be embodied in other specific forms without departing from the spirit or essential characteristics of the invention. Therefore, the embodiments should be considered in all respects as illustrative and non-restrictive, and the scope of the invention is defined by the appended claims, not the foregoing description, and all variations within the meaning and range of equivalents of the claims are intended to be included therein. Any reference sign in a claim should not be construed as limiting the claim to which it relates.

[0083] In addition, it should be understood that although this specification is described in terms of implementation methods, not every implementation method contains only one independent technical solution. This narrative method of the specification is only for the sake of clarity. Those skilled in the art should regard the specification as a whole. The technical solutions in each embodiment can also be appropriately combined to form other implementation methods that can be understood by those skilled in the art.

Claims

1. A method for preparing shrinkage-resistant and wrinkle-resistant cotton textile fabric, characterized in that: The following steps are involved: (1) Select long-staple cotton fibers that have been genetically modified to have higher fiber strength and uniform fiber diameter; (2) Ultrasonic-assisted enzymatic pretreatment of cotton fibers was performed. By controlling the ultrasonic power and enzyme concentration, a nano-scale microporous structure was formed on the fiber surface to enhance the binding force of the subsequent cross-linking agent; (3) preparing a treatment solution containing a novel bifunctional crosslinking agent, wherein the crosslinking agent comprises a reversible crosslinking group and a nanoscale catalyst carrier, wherein the crosslinking agent realizes inter-fiber crosslinking through dynamic covalent bonds and can partially break under specific circumstances to release stress; (4) Immersing the pretreated fabric in the treatment solution, using pulsed electric field assisted penetration technology to promote the crosslinking agent to uniformly penetrate the interior of the fiber, the immersion time being 3 to 15 minutes; (5) Treating the fiber surface with low-temperature plasma activation further enhances the bonding stability between the crosslinker and the fiber and the anti-wrinkle performance of the fabric; (6) Using a segmented temperature-controlled heat setting process, multi-stage heating treatment is performed in the range of 90°C to 140°C to control the time and temperature gradient, optimize the internal stress distribution of the fiber, and achieve excellent anti-shrinkage and anti-wrinkle effects; (7) Perform post-finishing treatment, which includes supercritical CO2 extraction and cleaning to remove unreacted residues and improve the soft feel and environmental performance of the fabric.

2. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The gene-edited long-staple cotton fiber regulates cellulose synthesis-related genes through CRISPR-Cas9 technology to improve fiber crystallinity and heat resistance.

3. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: In the ultrasonic-assisted enzymatic hydrolysis pretreatment step, the ultrasonic frequency is controlled at 20-40 kHz, the enzyme is a cellulase complex enzyme preparation, and the pretreatment time is 10-30 minutes.

4. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The novel bifunctional crosslinking agent is a polymer network structure containing a dynamic imine bond and a nano zinc oxide catalyst, and has both efficient crosslinking ability and self-repairing performance.

5. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The pulsed electric field assisted penetration technology uses an electric field strength of 0.5-2 kV / cm, a pulse width of 100-500 μs, and a frequency of 10-100 Hz to improve the penetration efficiency and uniformity of the crosslinking agent.

6. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The low-temperature plasma activation treatment uses oxygen or argon plasma, with a treatment time of 30 seconds to 3 minutes and a power of 50-150W.

7. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The segmented temperature-controlled heat setting process realizes multi-stage temperature curve control through an intelligent temperature control system, with the first stage being 90-110°C and the second stage being 120-140°C, each maintained for 1-3 minutes.

8. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The supercritical CO2 extraction conditions are a temperature of 35-45°C, a pressure of 10-15 MPa, and an extraction time of 20-40 minutes.

9. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The prepared cotton fabric has anti-wrinkle performance with a wrinkle recovery rate of ≥90% and a shrinkage rate of ≤2%, and has excellent air permeability and durability.

10. The method for preparing a shrinkage-resistant and wrinkle-resistant cotton textile fabric according to claim 1, characterized in that: The fabric also has a certain self-repair function. After microcracks are generated under stress, the fabric structure is repaired by breaking and reorganizing dynamic cross-linking bonds, thereby extending the service life of the fabric.

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