Preparation method of an anti-wrinkle and comfortable fabric
The pure cotton fabric is sorted through the quaternary ammonium salt-modified polysiloxane finishing solution, which solves the problem of insufficient anti-wrinkle and anti-bacterial properties in the existing technology, and achieves the improvement of the anti-wrinkle comfort performance of the fabric.
Patent Information
- Application Number
- CN202411541717.7
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-10-31
- Publication Date
- 2025-07-08
- Estimated Expiration
- 2044-10-31
AI Technical Summary
The prior art is difficult to maintain its antibacterial properties while improving the wrinkle resistance of cotton fabrics.
The pure cotton fabric is subjected to two-thrust and two-rolling and finishing with quaternary ammonium modified polysiloxane. The amino and carboxyl groups in the quaternary ammonium modified polysiloxane form hydrogen bonds with the cotton fibers, limit the deformation of the fiber molecular chain, and achieve antibacterial effects through electrostatic adsorption.
The fabrics prepared have good wrinkle and antibacterial properties, improving the moisture absorption and softness of the fabric.
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Figure CN119553505B_ABST
Abstract
Description
Technical Field
[0001] The present invention relates to the technical field of fabrics, and specifically to a preparation method of a wrinkle-resistant and comfortable fabric. Background Art
[0002] Cotton fiber is a natural cellulose fiber with good air permeability, moisture permeability and comfort performance. The cotton fabric prepared therefrom has the advantages of soft hand feeling, comfortable wearing and good air permeability, so it is loved by the majority of consumers. However, it is easy to wrinkle and deform after being washed with water, so it is necessary to carry out wrinkle-resistant finishing on pure cotton fabrics.
[0003] For example, the patent with the authorization publication number CN 107558199 B discloses a wrinkle-resistant finishing agent for cotton fabrics. The invention uses malic acid, maleic acid, softener, etc. as raw materials to prepare a wrinkle-resistant finishing agent for cotton fabrics. After the cotton fabric is finished with it, it has the advantages of good wrinkle-resistant effect, no formaldehyde release and not easy to fade, but its antibacterial performance is not improved.
[0004] For example, the patent with the authorization publication number CN 107287899 B discloses an antibacterial finishing method for cotton fabrics. The invention mixes a nano-zinc oxide composite solution and a quaternary ammonium salt polymer solution to obtain a zinc oxide-quaternary ammonium salt polymer composite antibacterial agent, and then configures it into an antibacterial finishing solution. The cotton fabric is padded with the finishing solution. The treated cotton fabric has a good antibacterial effect, but its wrinkle-resistant performance is not improved. Summary of the Invention
[0005] (1) Technical Problems to be Solved
[0006] In view of the deficiencies of the prior art, the present invention provides a preparation method of a wrinkle-resistant and comfortable fabric, and the prepared fabric has good wrinkle-resistant and comfortable performance as well as antibacterial performance.
[0007] (2) Technical Solutions
[0008] A preparation method of a wrinkle-resistant and comfortable fabric is as follows:
[0009] (1) Under a nitrogen atmosphere, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, methyltriethoxysilane, aminopropyltriethoxysilane, and polycarboxylic acid disilane gemini quaternary ammonium salt are added to a flask, stirred and dispersed, and reacted at 100-110 °C for 2-4 h. Then, the temperature is further raised to 130-140 °C and reacted for 1-2 h. After the reaction is completed, it is cooled to room temperature, subjected to vacuum distillation and drying to obtain quaternary ammonium salt-modified polysiloxane;
[0010] (2) Mix the quaternary ammonium salt modified polysiloxane and the emulsifier evenly, add them to deionized water and emulsify until the solid content is 30%, adjust the pH to 6 - 7 with acetic acid, stir and mix evenly to obtain the quaternary ammonium salt modified polysiloxane emulsion;
[0011] (3) At room temperature, add the quaternary ammonium salt modified polysiloxane emulsion to deionized water, stir and disperse to prepare a finishing solution, control the concentration to be 20 - 30 g / L, then add pure cotton fabric into it, and carry out two - dip two - roll finishing with a padding mangle, control the liquor pickup rate to be 80 - 100%, pre - dry at 100 °C for 5 min, bake at 150 °C for 1 - 3 min, and place it for 24 h under the conditions of 20 °C and 65% relative humidity to obtain the wrinkle - resistant and comfortable fabric.
[0012] Preferably, in the step (1), the mass ratio of octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, methyltriethoxysilane, aminopropyltriethoxysilane, and polycarboxyl di - silane gemini quaternary ammonium salt is 100:0.05 - 0.2:50 - 100:10 - 20:10 - 50.
[0013] Preferably, in the step (2), the mass ratio of the quaternary ammonium salt modified polysiloxane to the emulsifier is 100:40 - 60.
[0014] Preferably, in the step (2), the emulsifier is one of fatty alcohol polyoxyethylene ether 1350 and fatty alcohol polyoxyethylene ether 1390.
[0015] Preferably, in the step (1), the preparation method of the polycarboxyl di - silane gemini quaternary ammonium salt is as follows:
[0016] S1. Under a nitrogen atmosphere, add alkyl diamine and acrylonitrile to a methanol solvent, stir and react at room temperature for 36 - 48 h. After the reaction, carry out vacuum distillation to obtain intermediate 1;
[0017] S2. Under a nitrogen atmosphere, add intermediate 1 to a 50% sulfuric acid aqueous solution, stir and disperse, heat up to 110 - 120 °C, keep the temperature for 3 - 6 h. After the reaction, cool to room temperature, filter, wash with deionized water, and dry to obtain intermediate 2;
[0018] S3. Under a nitrogen atmosphere, add intermediate 2, γ - chloropropylmethyldimethoxysilane, and sodium iodide to an ethanol solvent, stir and disperse, react at 75 - 85 °C for 24 - 36 h. After the reaction, cool to room temperature, carry out suction filtration, vacuum distillation, and drying to obtain the polycarboxyl di - silane gemini quaternary ammonium salt.
[0019] Preferably, in the step S1, the molar ratio of alkyl diamine to acrylonitrile is 1:4 - 6.
[0020] Preferably, in S1, the structural formula of the alkylenediamine is NH2-R-NH2, where R = C n H 2n , and 2 ≤ n ≤ 6.
[0021] Preferably, in S3, the molar ratio of intermediate 2, γ-chloropropylmethyldimethoxysilane, and sodium iodide is 1:2 - 2.4:0.02 - 0.03.
[0022] (III) Beneficial technical effects
[0023] In the present invention, using alkylenediamine and acrylonitrile as raw materials, through an addition reaction, intermediate 1 is obtained. By hydrolyzing the cyano group contained therein in an aqueous sulfuric acid solution, intermediate 2 is obtained. Under the catalysis of sodium iodide, intermediate 2 and γ-chloropropylmethyldimethoxysilane undergo a quaternization reaction to obtain a multi-carboxyl disilane gemini quaternary ammonium salt. Using octamethylcyclotetrasiloxane, multi-carboxyl disilane gemini quaternary ammonium salt, etc. as raw materials, through base-catalyzed copolymerization, a quaternary ammonium salt-modified polysiloxane is obtained, which is then emulsified to prepare a finishing liquid. The pure cotton fabric is immersed therein, and through two-dip two-roll finishing, a wrinkle-resistant and comfortable fabric is obtained.
[0024] The finishing liquid prepared in the present invention contains polar groups such as amino groups and carboxyl groups. After the pure cotton fabric is finished, it can not only improve the moisture absorption performance of the pure cotton fabric, but also produce directional adsorption with the hydroxyl groups on the cotton fibers, form hydrogen bonds, and be fixed inside and on the surface of the fibers, restricting the deformation and movement of the cotton fiber molecular chains, thereby achieving the purpose of anti-wrinkle.
[0025] The polysiloxane skeleton prepared in the present invention is composed of a Si-O-Si structure. Its bond angle is large and the bond length is long, and it can rotate freely by 360 degrees. After the pure cotton fabric is finished, the polysiloxane chain segments can rotate and slip freely on the fiber surface, making the fabric have good soft and comfortable properties.
[0026] In addition, the finishing agent prepared in the present invention contains a quaternary ammonium salt structure with a positive charge. It can be adsorbed onto the surface of the negatively charged cell membrane through electrostatic adsorption, combine with the negatively charged substances on the cell membrane surface, destroy the cell membrane, and cause the loss of intracellular substances, thereby achieving the purpose of sterilization and antibacterial. The fabric prepared in the present invention has been experimentally verified to have good anti-wrinkle and comfortable properties as well as antibacterial properties. Description of the drawings
[0027] Figure 1 is the reaction route of the multi-carboxyl disilane gemini quaternary ammonium salt. Detailed implementation manners
[0028] "Preferred" in the present invention refers to embodiments of the present invention that can provide certain beneficial effects under certain circumstances. However, in the same or other circumstances, other embodiments may also be preferred. In addition, the description of one or more preferred embodiments does not imply that other embodiments are not available, nor is it intended to exclude other embodiments from the scope of the present invention.
[0029] Example 1
[0030] (1) Under a nitrogen atmosphere, 0.1 mol of ethylenediamine and 0.4 mol of acrylonitrile were added to a methanol solvent, and the mixture was stirred and reacted at room temperature for 48 h. After the reaction was completed, it was distilled under reduced pressure to obtain Intermediate 1.
[0031] (2) Under a nitrogen atmosphere, 0.2 mol of Intermediate 1 was added to a sulfuric acid aqueous solution with a mass fraction of 50%, stirred and dispersed, heated to 115 °C, and kept warm for reaction for 4 h. After the reaction was completed, it was cooled to room temperature, filtered, washed with deionized water, and dried to obtain Intermediate 2.
[0032] (3) Under a nitrogen atmosphere, 0.05 mol of Intermediate 2, 0.1 mol of γ-chloropropylmethyldimethoxysilane, and 0.001 mol of sodium iodide were added to an ethanol solvent, stirred and dispersed, and reacted at 80 °C for 36 h. After the reaction was completed, it was cooled to room temperature, suction filtered, distilled under reduced pressure, and dried to obtain a polycarboxy disilane gemini quaternary ammonium salt.
[0033] (4) Under a nitrogen atmosphere, 20 g of octamethylcyclotetrasiloxane, 0.02 g of tetramethylammonium hydroxide, 10 g of methyltriethoxysilane, 4 g of aminopropyltriethoxysilane, and 2 g of polycarboxy disilane gemini quaternary ammonium salt were added to a flask, stirred and dispersed, and reacted at 105 °C for 4 h. Then, the temperature was further raised to 130 °C and reacted for 2 h. After the reaction was completed, it was cooled to room temperature, distilled under reduced pressure, and dried to obtain a quaternary ammonium salt modified polysiloxane.
[0034] (5) 40 g of the quaternary ammonium salt modified polysiloxane and 24 g of fatty alcohol polyoxyethylene ether 1390 were mixed evenly, added to deionized water and emulsified until the solid content was 30%, and the pH was adjusted to 6 with acetic acid and stirred and mixed evenly to obtain a quaternary ammonium salt modified polysiloxane emulsion.
[0035] (6) At room temperature, the quaternary ammonium salt modified polysiloxane emulsion was added to deionized water, stirred and dispersed to prepare a finishing solution with a controlled concentration of 20 g / L. Then, pure cotton fabric was added thereto, and two-dip two-roll finishing was carried out using a padding mangle, with the controlled liquor pickup rate being 80%. It was pre-dried at 100 °C for 5 min and baked at 150 °C for 3 min, and placed for 24 h under the conditions of 20 °C and a relative humidity of 65% to obtain a wrinkle-resistant and comfortable fabric.
[0036] Example 2
[0037] (1) Under a nitrogen atmosphere, 0.1 mol of 1,3 - propanediamine and 0.6 mol of acrylonitrile were added to a methanol solvent, and stirred at room temperature for 42 h. After the reaction, distillation under reduced pressure was carried out to obtain Intermediate 1.
[0038] (2) Under a nitrogen atmosphere, 0.2 mol of Intermediate 1 was added to an aqueous sulfuric acid solution with a mass fraction of 50%, stirred and dispersed, heated to 115 °C, and kept at this temperature for reaction for 5 h. After the reaction, the temperature was cooled to room temperature, filtered, washed with deionized water, and dried to obtain Intermediate 2.
[0039] (3) Under a nitrogen atmosphere, 0.05 mol of Intermediate 2, 0.1 mol of γ - chloropropylmethyldimethoxysilane, and 0.0015 mol of sodium iodide were added to an ethanol solvent, stirred and dispersed, and reacted at 80 °C for 30 h. After the reaction, it was cooled to room temperature, suction - filtered, distilled under reduced pressure, and dried to obtain a polycarboxy disilane gemini quaternary ammonium salt.
[0040] (4) Under a nitrogen atmosphere, 20 g of octamethylcyclotetrasiloxane, 0.01 g of tetramethylammonium hydroxide, 12 g of methyltriethoxysilane, 2 g of aminopropyltriethoxysilane, and 4 g of polycarboxy disilane gemini quaternary ammonium salt were added to a flask, stirred and dispersed, and reacted at 105 °C for 4 h. Then it was further heated to 135 °C and reacted for 2 h. After the reaction, it was cooled to room temperature, distilled under reduced pressure, and dried to obtain a quaternary ammonium salt - modified polysiloxane.
[0041] (5) 40 g of the quaternary ammonium salt - modified polysiloxane and 20 g of fatty alcohol polyoxyethylene ether 1390 were mixed evenly, added to deionized water and emulsified until the solid content was 30%, and the pH was adjusted to 6 with acetic acid, then stirred and mixed evenly to obtain a quaternary ammonium salt - modified polysiloxane emulsion.
[0042] (6) At room temperature, the quaternary ammonium salt - modified polysiloxane emulsion was added to deionized water, stirred and dispersed to prepare a finishing solution with a controlled concentration of 23 g / L. Then, pure cotton fabric was added to it, and two - dip and two - nip finishing was carried out using a padding mangle, with a controlled liquor - pick - up rate of 90%. It was pre - dried at 100 °C for 5 min and baked at 150 °C for 2 min, and placed for 24 h at 20 °C and a relative humidity of 65% to obtain a wrinkle - resistant and comfortable fabric.
[0043] Example 3
[0044] (1) Under a nitrogen atmosphere, 0.1 mol of 1,4 - butanediamine and 0.5 mol of acrylonitrile were added to a methanol solvent, and stirred at room temperature for 36 h. After the reaction, distillation under reduced pressure was carried out to obtain Intermediate 1.
[0045] (2) Under a nitrogen atmosphere, 0.2 mol of intermediate 1 was added to an aqueous sulfuric acid solution with a mass fraction of 50%, stirred and dispersed, heated to 110 °C, and kept at this temperature for reaction for 4 h. After the reaction, it was cooled to room temperature, filtered, washed with deionized water, and dried to obtain intermediate 2.
[0046] (3) Under a nitrogen atmosphere, 0.05 mol of intermediate 2, 0.1 mol of γ-chloropropylmethyldimethoxysilane, and 0.001 mol of sodium iodide were added to an ethanol solvent, stirred and dispersed, and reacted at 75 °C for 36 h. After the reaction, it was cooled to room temperature, suction filtered, distilled under reduced pressure, and dried to obtain a multi-carboxyl disilane gemini quaternary ammonium salt.
[0047] (4) Under a nitrogen atmosphere, 20 g of octamethylcyclotetrasiloxane, 0.01 g of tetramethylammonium hydroxide, 15 g of methyltriethoxysilane, 4 g of aminopropyltriethoxysilane, and 6 g of the multi-carboxyl disilane gemini quaternary ammonium salt were added to a flask, stirred and dispersed, and reacted at 100 °C for 4 h. Then it was heated to 140 °C and reacted for 1 h. After the reaction, it was cooled to room temperature, distilled under reduced pressure, and dried to obtain a quaternary ammonium salt modified polysiloxane.
[0048] (5) 40 g of the quaternary ammonium salt modified polysiloxane and 16 g of fatty alcohol polyoxyethylene ether 1350 were mixed evenly, added to deionized water and emulsified until the solid content was 30%, and the pH was adjusted to 7 with acetic acid, and then stirred and mixed evenly to obtain a quaternary ammonium salt modified polysiloxane emulsion.
[0049] (6) At room temperature, the quaternary ammonium salt modified polysiloxane emulsion was added to deionized water, stirred and dispersed to prepare a finishing solution with a concentration of 25 g / L. Then pure cotton fabric was added thereto, and two-dip two-roll finishing was carried out using a padding mangle, controlling the liquor pickup rate to be 90%. It was pre-dried at 100 °C for 5 min and baked at 150 °C for 3 min, and then placed at 20 °C and a relative humidity of 65% for 24 h to obtain a wrinkle-resistant and comfortable fabric.
[0050] Example 4
[0051] (1) Under a nitrogen atmosphere, 0.1 mol of 1,5-pentanediamine and 0.5 mol of acrylonitrile were added to a methanol solvent, and stirred and reacted at room temperature for 40 h. After the reaction, it was distilled under reduced pressure to obtain intermediate 1.
[0052] (2) Under a nitrogen atmosphere, 0.2 mol of intermediate 1 was added to an aqueous sulfuric acid solution with a mass fraction of 50%, stirred and dispersed, heated to 115 °C, and kept at this temperature for reaction for 6 h. After the reaction, it was cooled to room temperature, filtered, washed with deionized water, and dried to obtain intermediate 2.
[0053] (3) Under a nitrogen atmosphere, 0.05 mol of intermediate 2, 0.12 mol of γ-chloropropylmethyldimethoxysilane, and 0.0015 mol of sodium iodide were added to an ethanol solvent, stirred and dispersed, and reacted at 80 °C for 36 h. After the reaction, it was cooled to room temperature, filtered by suction, distilled under reduced pressure, and dried to obtain a polycarboxy disilane gemini quaternary ammonium salt.
[0054] (4) Under a nitrogen atmosphere, 20 g of octamethylcyclotetrasiloxane, 0.04 g of tetramethylammonium hydroxide, 18 g of methyltriethoxysilane, 3 g of aminopropyltriethoxysilane, and 8 g of polycarboxy disilane gemini quaternary ammonium salt were added to a flask, stirred and dispersed, and reacted at 110 °C for 2 h. Then the temperature was raised to 130 °C and reacted for 2 h. After the reaction, it was cooled to room temperature, distilled under reduced pressure, and dried to obtain a quaternary ammonium salt modified polysiloxane.
[0055] (5) 40 g of the quaternary ammonium salt modified polysiloxane and 20 g of fatty alcohol polyoxyethylene ether 1390 were mixed evenly, added to deionized water and emulsified until the solid content was 30%. The pH was adjusted to 6 with acetic acid, and stirred and mixed evenly to obtain a quaternary ammonium salt modified polysiloxane emulsion.
[0056] (6) At room temperature, the quaternary ammonium salt modified polysiloxane emulsion was added to deionized water, stirred and dispersed to prepare a finishing solution with a concentration controlled at 28 g / L. Then pure cotton fabric was added to it, and two-dip two-roll finishing was carried out using a padding mangle, with the liquor pickup rate controlled at 100%. It was pre-dried at 100 °C for 5 min and baked at 150 °C for 1 min. It was placed for 24 h at 20 °C and a relative humidity of 65% to obtain a wrinkle-resistant and comfortable fabric.
[0057] Example 5
[0058] (1) Under a nitrogen atmosphere, 0.1 mol of 1,6-hexanediamine and 0.5 mol of acrylonitrile were added to a methanol solvent, and stirred and reacted at room temperature for 48 h. After the reaction, it was distilled under reduced pressure to obtain intermediate 1.
[0059] (2) Under a nitrogen atmosphere, 0.2 mol of intermediate 1 was added to a sulfuric acid aqueous solution with a mass fraction of 50%, stirred and dispersed, heated to 120 °C, and kept warm for 3 h. After the reaction, it was cooled to room temperature, filtered, washed with deionized water, and dried to obtain intermediate 2.
[0060] (3) Under a nitrogen atmosphere, 0.05 mol of intermediate 2, 0.1 mol of γ-chloropropylmethyldimethoxysilane, and 0.001 mol of sodium iodide were added to an ethanol solvent, stirred and dispersed, and reacted at 85 °C for 24 h. After the reaction, it was cooled to room temperature, filtered by suction, distilled under reduced pressure, and dried to obtain a polycarboxy disilane gemini quaternary ammonium salt.
[0061] (4) Under a nitrogen atmosphere, 20 g of octamethylcyclotetrasiloxane, 0.01 g of tetramethylammonium hydroxide, 20 g of methyltriethoxysilane, 2 g of aminopropyltriethoxysilane, and 10 g of polycarboxylic disilane gemini quaternary ammonium salt were added to a flask, stirred and dispersed, reacted at 100 °C for 3 h, then heated to 135 °C and reacted for 2 h. After the reaction, it was cooled to room temperature, subjected to vacuum distillation and drying to obtain quaternary ammonium salt-modified polysiloxane.
[0062] (5) 40 g of quaternary ammonium salt-modified polysiloxane and 20 g of fatty alcohol polyoxyethylene ether 1350 were mixed evenly, added to deionized water and emulsified until the solid content was 30%. The pH was adjusted to 7 with acetic acid, and stirred and mixed evenly to obtain a quaternary ammonium salt-modified polysiloxane emulsion.
[0063] (6) At room temperature, the quaternary ammonium salt-modified polysiloxane emulsion was added to deionized water, stirred and dispersed to prepare a finishing solution, with the concentration controlled at 30 g / L. Then, pure cotton fabric was added, and two-dip two-roll finishing was carried out using a padder, with the liquor pickup rate controlled at 100%. It was pre-dried at 100 °C for 5 min and baked at 150 °C for 2 min. It was placed for 24 h at 20 °C and a relative humidity of 65% to obtain a wrinkle-resistant and comfortable fabric.
[0064] Referring to GB / T3819-1977, using a fabric crease recovery tester, the wrinkle resistance of the fabric was tested. The fabric size was 40 mm × 40 mm, with ten warp and ten weft. After equilibration for 4 h at 20 °C and a relative humidity of 65%, the crease recovery angle WRA value (warp + weft) was used as the fabric crease recovery performance index.
[0065] Table 1:
[0066] WRA(°) Example 1 245 Example 2 264 Example 3 272 Example 4 278 Example 5 274 Comparative Example 1 233
[0067] Comparative Example 1 was a pure cotton fabric finished with a commercially available finishing solution, and its finishing process was the same as that of Example 1.
[0068] The larger the crease recovery angle, the better the wrinkle resistance of the fabric. As shown in the table, the crease recovery angle of the example was larger than that of Comparative Example 1, and in the examples, as the amount of the finishing solution increased, the crease recovery angle became larger, and the maximum could reach 278°.
[0069] The handle of the fabric was tested using a fabric style tester. The fabric was equilibrated for 24 h at 20 °C and a relative humidity of 65%. Three circular specimens with a diameter of 10 cm were selected at different positions on the same fabric to test softness and smoothness. The test result value range was 0-100, and the larger the value of each index, the stronger the property of the sample.
[0070] Table 2:
[0071] Flexibility Smoothness Example 1 80.26 86.40 Example 2 84.33 89.42 Example 3 86.92 93.28 Example 4 89.64 95.16 Example 5 91.25 95.10 Comparative Example 1 76.75 81.44
[0072] Comparative Example 1 is a pure cotton fabric finished with a commercially available finishing liquid, and its finishing process is the same as that of Example 1.
[0073] As can be seen from the table, the pure cotton fabric prepared by the present invention has good soft and comfortable properties.
[0074] Referring to GB / T20944.3-2008, the antibacterial properties of the pure cotton fabric were tested, and the test strains were Escherichia coli and Staphylococcus aureus.
[0075] Table 3:
[0076] Bacteriostatic rate (%) Example 1 94.3 Example 2 98.6 Example 3 99.9 Example 4 99.9 Example 5 99.9
[0077] As can be seen from the table, the fabric prepared by the present invention has good antibacterial effects, and the highest bacteriostatic rate can reach 99.9%.
[0078] The above are only the preferred embodiments of the present invention. It should be noted that for those of ordinary skill in the art, without departing from the principle of the present invention, several improvements and refinements can be made, and these improvements and refinements should also be regarded as the protection scope of the present invention.
Claims
1. A method for preparing an anti-wrinkle and comfortable fabric, characterized in that, The preparation method is as follows: (1) Under a nitrogen atmosphere, octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, methyltriethoxysilane, aminopropyltriethoxysilane, and polycarboxy disilane gemini quaternary ammonium salt are added to a flask, stirred and dispersed, reacted at 100 - 110 °C for 2 - 4 h, then further heated to 130 - 140 °C and reacted for 1 - 2 h. After the reaction is completed, it is cooled to room temperature, subjected to vacuum distillation and drying to obtain quaternary ammonium salt modified polysiloxane; (2) The quaternary ammonium salt modified polysiloxane and the emulsifier are mixed evenly, deionized water is added thereto and emulsified until the solid content is 30%, and the pH is adjusted to 6 - 7 with acetic acid, and then stirred and mixed evenly to obtain a quaternary ammonium salt modified polysiloxane emulsion; (3) At room temperature, the quaternary ammonium salt modified polysiloxane emulsion is added to deionized water, stirred and dispersed to prepare a finishing solution, with the concentration controlled at 20 - 30 g / L. Then, pure cotton fabric is added thereto, and two - dip two - nip finishing is carried out using a padding mangle, with the nip - pick - up rate controlled at 80 - 100%, pre - dried at 100 °C for 5 min, baked at 150 °C for 1 - 3 min, and placed for 24 h at 20 °C and a relative humidity of 65% to obtain a wrinkle - resistant and comfortable fabric; The preparation method of the polycarboxy disilane gemini quaternary ammonium salt is as follows: S1. Under a nitrogen atmosphere, alkyl diamine and acrylonitrile are added to a methanol solvent, and stirred and reacted at room temperature for 36 - 48 h. After the reaction is completed, vacuum distillation is carried out to obtain intermediate 1; S2. Under a nitrogen atmosphere, intermediate 1 is added to a 50% by mass sulfuric acid aqueous solution, stirred and dispersed, heated to 110 - 120 °C, and kept warm for 3 - 6 h. After the reaction is completed, it is cooled to room temperature, filtered, washed with deionized water, and dried to obtain intermediate 2; S3. Under a nitrogen atmosphere, intermediate 2, γ - chloropropylmethyldimethoxysilane, and sodium iodide are added to an ethanol solvent, stirred and dispersed, reacted at 75 - 85 °C for 24 - 36 h. After the reaction is completed, it is cooled to room temperature, suction - filtered, vacuum - distilled, and dried to obtain polycarboxy disilane gemini quaternary ammonium salt.
2. The preparation method of the anti-wrinkle and comfortable fabric according to claim 1, wherein In the step (1), the mass ratio of octamethylcyclotetrasiloxane, tetramethylammonium hydroxide, methyltriethoxysilane, aminopropyltriethoxysilane, and polycarboxy disilane gemini quaternary ammonium salt is 100:0.05 - 0.2:50 - 100:10 - 20:10 - 50.
3. The preparation method of the anti-wrinkle and comfortable fabric according to claim 1, characterized in that, In the step (2), the mass ratio of the quaternary ammonium salt modified polysiloxane to the emulsifier is 100:40 - 60.
4. The preparation method of the wrinkle-resistant and comfortable fabric according to claim 1, characterized in that, In the step (2), the emulsifier is one of fatty alcohol polyoxyethylene ether 1350 and fatty alcohol polyoxyethylene ether 1390.
5. The preparation method of the anti-wrinkle and comfortable fabric according to claim 1, characterized in that, In the step S1, the molar ratio of alkyl diamine to acrylonitrile is 1:4 - 6.
6. The preparation method of the anti-wrinkle and comfortable fabric according to claim 1, characterized in that, In the above S1, the structural formula of the alkylenediamine is NH2-R-NH2, where R = C n H 2n , and 2 ≤ n ≤ 6.
7. The preparation method of the wrinkle-resistant and comfortable fabric according to claim 1, characterized in that, In the step S3, the molar ratio of intermediate 2, γ - chloropropylmethyldimethoxysilane, and sodium iodide is 1:2 - 2.4:0.02 - 0.03.
Citation Information
Patent Citations
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CN107558199B
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