Preparation method of hydrophobic breathable fabric

Abstract

The invention relates to the technical field of fabrics, and discloses a preparation method of a hydrophobic breathable fabric, which comprises the following steps: taking p-perfluorononenoxy benzene sulfonyl chloride, 3, 5-bis-aminomethyl-phenol, chloropropene and the like as raw materials, and carrying out amidation reaction and substitution reaction to obtain an intermediate 2; according to the method, N, N-dimethyl-N-dodecyl tertiary amine and chloropropene are taken as raw materials, and the allyl dodecyl dimethyl ammonium chloride is obtained through quaternization reaction. And carrying out copolymerization on octadecyl acrylate, the intermediate 2, allyl dodecyl dimethyl ammonium chloride and the like under the initiation of azodiisobutyronitrile to obtain the fluorine-containing modified polyacrylate finishing agent. Immersing the fabric into the fluorine-containing modified polyacrylate finishing agent, and carrying out two times of dipping and two times of rolling, pre-drying and baking to obtain the hydrophobic breathable fabric. The prepared fabric has good antibacterial, breathable and hydrophobic effects.

Description

Technical Field

[0001] The invention relates to the technical field of fabrics, and in particular to a method for preparing a hydrophobic and breathable fabric. Background Art

[0002] With the diversified development of lifestyles and the improvement of people's living standards, the functions of traditional fabrics can no longer meet people's life needs. People are paying more and more attention to the needs for various functions of fabrics. Therefore, various functional textiles have received widespread attention and long-term development.

[0003] Hydrophobic fabrics are widely used in the field of clothing. In addition, people are now demanding higher and higher performance from hydrophobic clothing. People are not satisfied with the improvement of hydrophobic properties alone. Therefore, there is great potential for the development of hydrophobic fabrics. Fabric finishing agents are a type of finishing aid in textile production. When applied to the surface of a fabric, the surface properties of the fabric change dramatically, thus giving the fabric special functions.

[0004] For example, the patent application publication number CN 117403370 A discloses a waterproof, oil-proof and anti-fouling fabric and a preparation method thereof. The invention uses polyester fiber and spandex fiber to make A yarn through a twisting process, and modified activated carbon fiber and nylon fiber are blended to make B yarn. After weaving, a base fabric is obtained, which is then subjected to a series of treatments. The final fabric has good waterproof and breathable properties. Summary of the invention

[0005] 1. Technical issues to be solved

[0006] In view of the deficiencies in the prior art, the present invention provides a method for preparing a hydrophobic and breathable fabric. The prepared fabric is finished with a fluorine-containing modified polyacrylate finishing agent and has good hydrophobicity, breathability and antibacterial properties.

[0007] (II) Technical solution

[0008] A method for preparing a hydrophobic and breathable fabric, the preparation method is as follows:

[0009] Step (1), add octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, allyl dodecyl dimethyl ammonium chloride, and azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 70-90° C., react for 2-5 hours, then add deionized water, continue stirring for 2-4 hours, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0010] Step (2), immersing the fabric in a fluorine-containing modified polyacrylate finishing agent, wherein the material of the fabric is one of polyester, spandex, nylon, and cotton, and undergoing two immersions and two rollings, controlling the rolling rate to be 65-80%, pre-baking the fabric at 100° C. for 5 minutes, then heating it to 140-180° C., and baking it for 5 minutes to obtain a hydrophobic and breathable fabric.

[0011] Preferably, in step (1), the mass ratio of octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, and allyl dodecyl dimethyl ammonium chloride is 1 g: (3-6) g: (0.3-0.8) g: (4-8) g: (2-6) g.

[0012] Preferably, in step (1), the mass of azobisisobutyronitrile is 1-3% of the total mass of octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, and allyldodecyldimethylammonium chloride.

[0013] Preferably, in step (2), the mass concentration of the fluorine-modified polyacrylate finishing agent is 20-100 g / L.

[0014] Preferably, in step (1), the preparation method of intermediate 2 is:

[0015] S1. Add p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 3,5-bis-aminomethyl-phenol, stir and react at 80-95°C for 2-5h. After the reaction, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0016] S2. Add intermediate 1, allyl chloride and cesium carbonate to acetonitrile solvent, stir and disperse, heat to 70-80°C, react for 5-12 hours. After the reaction, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with deionized water, and dry to obtain intermediate 2.

[0017] Preferably, in S1, the molar ratio of p-perfluorononenyloxybenzenesulfonyl chloride to 3,5-bis-aminomethyl-phenol is 2-2.5:1.

[0018] Preferably, in S2, the molar ratio of intermediate 1, propylene chloride and cesium carbonate is 1:1-1.5:1-1.5.

[0019] Preferably, in the step (1), the preparation method of allyl dodecyl dimethyl ammonium chloride is: adding N, N-dimethyl-N-dodecyl tertiary amine to an ether solvent, stirring and dispersing, then adding allyl chloride thereto, stirring and reacting at 25-30° C. for 3-6 hours, and after the reaction is completed, washing with ether and drying to obtain allyl dodecyl dimethyl ammonium chloride.

[0020] Preferably, the molar ratio of the N,N-dimethyl-N-dodecyl tertiary amine to allyl chloride is 1:0.8-1.2.

[0021] (III) Beneficial technical effects

[0022] The present invention uses p-perfluorononenyloxybenzenesulfonyl chloride and 3,5-bis-aminomethyl-phenol as raw materials, undergoes an amidation reaction, and then undergoes a substitution reaction with allyl chloride under the catalysis of cesium carbonate to obtain intermediate 2. N,N-dimethyl-N-dodecyl tertiary amine and allyl chloride are subjected to a quaternization reaction to obtain allyl dodecyl dimethyl ammonium chloride. Octadecanyl acrylate is copolymerized with intermediate 2, allyl dodecyl dimethyl ammonium chloride, etc. under the initiation of azobisisobutyronitrile to obtain a fluorine-containing modified polyacrylate finishing agent. The fabric is immersed in the fluorine-containing modified polyacrylate finishing agent, and after two immersions and two rollings, pre-baking and baking, a hydrophobic and breathable fabric is obtained.

[0023] The fabric prepared by the present invention contains a fluorine-containing carbon chain, which is added to the fabric. Since a large amount of fluorine exists on the surface of the fabric, the surface free energy of the fabric is reduced, thereby improving the hydrophobicity of the fabric. In addition, the finishing agent prepared by the present invention contains a large amount of alkyl long chains. After the fabric is finished, a lipid film can be formed on the surface of the fabric, which has good hydrophobicity, further improving the hydrophobicity of the fabric. In addition, since the alkyl long chain has a good degree of freedom, adding it to the fabric can improve the air permeability of the fabric. In addition, the finishing agent prepared by the present invention contains a quaternary ammonium salt, which is a good antibacterial structure. Adding it to the fabric can improve the antibacterial performance of the fabric. The fabric prepared by the present invention has good antibacterial, breathable and hydrophobic effects. BRIEF DESCRIPTION OF THE DRAWINGS

[0024] Figure 1 is the reaction formula of intermediate 2;

[0025] Figure 2 It is the reaction formula of allyl dodecyl dimethyl ammonium chloride. DETAILED DESCRIPTION

[0026] The specific embodiments of the present invention are further described below. It should be noted that the description of these embodiments is used to help understand the present invention, but does not constitute a limitation of the present invention. In addition, the technical features involved in each embodiment of the present invention described below can be combined with each other as long as they do not conflict with each other.

[0027] Example 1

[0028] (1) Add 50 mmol of p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 20 mmol of 3,5-bis-aminomethyl-phenol, stir and react at 85° C. for 4 h. After the reaction is completed, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0029] (2) 10 mmol of intermediate 1, 12 mmol of allyl chloride and 10 mmol of cesium carbonate were added to acetonitrile solvent, stirred and dispersed, heated to 75°C, and reacted for 6 hours. After the reaction was completed, deionized water was added, stirred, allowed to stand for stratification, the organic layer was taken, distilled under reduced pressure, washed with deionized water, and dried to obtain intermediate 2.

[0030] (3) Add 50 mmol of N,N-dimethyl-N-dodecyl tertiary amine to ether solvent, stir and disperse, then add 60 mmol of allyl chloride, stir and react at 30° C. for 5 hours. After the reaction is completed, wash with ether and dry to obtain allyl dodecyl dimethyl ammonium chloride.

[0031] (4) Add 2 g of octadecyl acrylate, 8 g of methyl methacrylate, 1.5 g of hydroxyethyl acrylate, 8 g of intermediate 2, 4 g of allyl dodecyl dimethyl ammonium chloride, and 1.2 g of azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 80°C, react for 4 h, add deionized water, continue stirring for 2 h, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0032] (5) The polyester fabric is immersed in a fluorine-modified polyacrylate finishing agent with a mass concentration of 20 g / L, and after two immersions and two rollings, the rolling rate is controlled to be 75%. The fabric sample is placed at 100°C for pre-baking for 5 minutes, and then the temperature is raised to 160°C and baked for 5 minutes to obtain a hydrophobic and breathable fabric.

[0033] Example 2

[0034] (1) Add 40 mmol of p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 20 mmol of 3,5-bis-aminomethyl-phenol, stir and react at 95° C. for 5 h. After the reaction is completed, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0035] (2) 10 mmol of intermediate 1, 15 mmol of allyl chloride and 15 mmol of cesium carbonate were added to acetonitrile solvent, stirred and dispersed, heated to 80°C, and reacted for 12 hours. After the reaction was completed, deionized water was added, stirred, allowed to stand for stratification, the organic layer was taken, distilled under reduced pressure, washed with deionized water, and dried to obtain intermediate 2.

[0036] (3) Add 50 mmol of N,N-dimethyl-N-dodecyl tertiary amine to ether solvent, stir and disperse, then add 50 mmol of allyl chloride, stir and react at 25° C. for 6 hours. After the reaction is completed, wash with ether and dry to obtain allyl dodecyl dimethyl ammonium chloride.

[0037] (4) Add 2 g of octadecyl acrylate, 8 g of methyl methacrylate, 1 g of hydroxyethyl acrylate, 10 g of intermediate 2, 6 g of allyl dodecyl dimethyl ammonium chloride, and 1 g of azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 80°C, react for 4 h, add deionized water, continue stirring for 3 h, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0038] (5) The polyester fabric is immersed in a fluorine-modified polyacrylate finishing agent with a mass concentration of 40 g / L, and after two immersions and two rollings, the rolling rate is controlled to be 70%. The fabric sample is placed at 100°C for pre-baking for 5 minutes, and then the temperature is increased to 150°C and baked for 5 minutes to obtain a hydrophobic and breathable fabric.

[0039] Example 3

[0040] (1) Add 45 mmol of p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 20 mmol of 3,5-bis-aminomethyl-phenol, stir and react at 80° C. for 2 h. After the reaction is completed, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0041] (2) 10 mmol of intermediate 1, 10 mmol of allyl chloride and 12 mmol of cesium carbonate were added to acetonitrile solvent, stirred and dispersed, heated to 70°C, and reacted for 8 hours. After the reaction was completed, deionized water was added, stirred, allowed to stand for stratification, the organic layer was taken, distilled under reduced pressure, washed with deionized water, and dried to obtain intermediate 2.

[0042] (3) Add 50 mmol of N,N-dimethyl-N-dodecyl tertiary amine to ether solvent, stir and disperse, then add 40 mmol of allyl chloride, stir and react at 30° C. for 3 h. After the reaction is completed, wash with ether and dry to obtain allyl dodecyl dimethyl ammonium chloride.

[0043] (4) Add 2 g of octadecyl acrylate, 12 g of methyl methacrylate, 1.6 g of hydroxyethyl acrylate, 12 g of intermediate 2, 8 g of allyl dodecyl dimethyl ammonium chloride, and 0.2 g of azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 90°C, react for 4 h, add deionized water, continue stirring for 3 h, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0044] (5) The polyester fabric was immersed in a fluorine-modified polyacrylate finishing agent with a mass concentration of 60 g / L, and after two immersions and two rollings, the rolling rate was controlled to be 65%. The fabric sample was pre-baked at 100°C for 5 minutes, and then the temperature was raised to 140°C and baked for 5 minutes to obtain a hydrophobic and breathable fabric.

[0045] Example 4

[0046] (1) Add 45 mmol of p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 20 mmol of 3,5-bis-aminomethyl-phenol, stir and react at 85° C. for 3 h. After the reaction is completed, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0047] (2) 10 mmol of intermediate 1, 12 mmol of allyl chloride and 15 mmol of cesium carbonate were added to acetonitrile solvent, stirred and dispersed, heated to 80°C, and reacted for 5 hours. After the reaction was completed, deionized water was added, stirred, allowed to stand for stratification, the organic layer was taken, distilled under reduced pressure, washed with deionized water, and dried to obtain intermediate 2.

[0048] (3) Add 50 mmol of N,N-dimethyl-N-dodecyl tertiary amine to ether solvent, stir and disperse, then add 50 mmol of allyl chloride, stir and react at 30° C. for 5 h. After the reaction is completed, wash with ether and dry to obtain allyl dodecyl dimethyl ammonium chloride.

[0049] (4) Add 2 g of octadecyl acrylate, 10 g of methyl methacrylate, 0.6 g of hydroxyethyl acrylate, 14 g of intermediate 2, 10 g of allyl dodecyl dimethyl ammonium chloride, and 1 g of azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 70°C, react for 5 h, add deionized water, continue stirring for 2 h, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0050] (5) The polyester fabric is immersed in a fluorine-modified polyacrylate finishing agent with a mass concentration of 80 g / L, and after two immersions and two rollings, the rolling rate is controlled to be 70%. The fabric sample is placed at 100°C for pre-baking for 5 minutes, and then the temperature is raised to 180°C, and the shape is fixed and baked for 5 minutes to obtain a hydrophobic and breathable fabric.

[0051] Example 5

[0052] (1) Add 45 mmol of p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stir and disperse, then add 20 mmol of 3,5-bis-aminomethyl-phenol, stir and react at 95° C. for 5 h. After the reaction is completed, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with ethanol, and dry to obtain intermediate 1.

[0053] (2) 10 mmol of intermediate 1, 14 mmol of allyl chloride and 12 mmol of cesium carbonate were added to acetonitrile solvent, stirred and dispersed, heated to 80°C, and reacted for 12 hours. After the reaction was completed, deionized water was added, stirred, allowed to stand for stratification, the organic layer was taken, distilled under reduced pressure, washed with deionized water, and dried to obtain intermediate 2.

[0054] (3) Add 50 mmol of N,N-dimethyl-N-dodecyl tertiary amine to ether solvent, stir and disperse, then add 46 mmol of allyl chloride, stir and react at 30° C. for 5 h. After the reaction is completed, wash with ether and dry to obtain allyl dodecyl dimethyl ammonium chloride.

[0055] (4) Add 2 g of octadecyl acrylate, 6 g of methyl methacrylate, 1 g of hydroxyethyl acrylate, 16 g of intermediate 2, 12 g of allyl dodecyl dimethyl ammonium chloride, and 1.3 g of azobisisobutyronitrile to N,N-dimethylformamide solvent, stir and disperse, heat to 80°C, react for 2 h, add deionized water, continue stirring for 4 h, and cool to room temperature to obtain a fluorine-modified polyacrylate finishing agent.

[0056] (5) The polyester fabric is immersed in a fluorine-modified polyacrylate finishing agent with a mass concentration of 100 g / L, and after two immersions and two rollings, the rolling rate is controlled to be 80%, and the fabric pattern is pre-baked at 100°C for 5 minutes, and then the temperature is increased to 150°C, and the shaping and baking are performed for 5 minutes to obtain a hydrophobic and breathable fabric.

[0057] Refer to GB / T4745-2012 for waterproof grade test. Test water temperature is 25℃, water flow rate is 100mL / min, spray time is 10min, leave for 1min, observe the surface condition of fabric for rating. Waterproof grade: Grade 1 means the whole surface is wetted; Grade 2 means partial wetted; Grade 3 means part of the sample is stained with water droplets; Grade 4 means large water droplets are formed; Grade 5 means small water droplets drip quickly.

[0058] The air permeability test was carried out according to GB / T8629-2001, the fabric size was 20cm×20cm, and the pressure drop was 100Pa.

[0059] Waterproof grade / level Air permeability / (mm / s) Example 1 4 55.84 Example 2 4 58.16 Example 3 4-5 62.30 Example 4 5 65.79 Example 5 5 67.03 Comparative Example 1 1 45.62

[0060] Comparative Example 1 is an unfinished polyester fabric.

[0061] It can be seen from the table that the fabric prepared by the present invention has good hydrophobicity and air permeability.

[0062] The fabric was cut into small discs with a diameter of 6 mm, and placed in a sterile container after ultraviolet sterilization. Escherichia coli and Staphylococcus aureus were inoculated in nutrient broth and cultured at 37°C for 12 h. The bacterial solution was diluted and evenly spread on a nutrient agar plate. The fabric disc was placed on the plate and cultured at 37°C for 24 h. The diameter of the inhibition zone was measured with a vernier caliper.

[0063]

[0064] Comparative Example 1 is an unfinished polyester fabric.

[0065] It can be seen from the table that the fabric prepared by the present invention has good antibacterial properties.

[0066] The above implementation modes are only used to illustrate the present invention, but not to limit the present invention. Ordinary technicians in the relevant technical field can make various changes and modifications without departing from the spirit and scope of the present invention. Therefore, all equivalent technical solutions also belong to the scope of the present invention. The patent protection scope of the present invention should be defined by the claims.

Claims

1. A method for preparing a hydrophobic and breathable fabric, characterized in that: The preparation method is as follows: Step (1), adding octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, allyl dodecyl dimethyl ammonium chloride, and azobisisobutyronitrile to N,N-dimethylformamide solvent, stirring and dispersing, heating to 70-90° C., reacting for 2-5 hours, then adding deionized water, continuing stirring for 2-4 hours, and cooling to room temperature to obtain a fluorine-modified polyacrylate finishing agent; Step (2), immersing the fabric in a fluorine-containing modified polyacrylate finishing agent, performing two immersions and two rollings, controlling the rolling rate to be 65-80%, pre-baking the fabric at 100°C for 5 minutes, then heating to 140-180°C, setting and baking for 5 minutes, to obtain a hydrophobic and breathable fabric.

2. The method for preparing the hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (1), the mass ratio of octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, and allyl dodecyl dimethyl ammonium chloride is 1 g: (3-6) g: (0.3-0.8) g: (4-8) g: (2-6) g.

3. The method for preparing the hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (1), the mass of azobisisobutyronitrile is 1-3% of the total mass of octadecyl acrylate, methyl methacrylate, hydroxyethyl acrylate, intermediate 2, and allyldodecyldimethylammonium chloride.

4. The method for preparing the hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (2), the mass concentration of the fluorine-modified polyacrylate finishing agent is 20-100 g / L.

5. The method for preparing the hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (1), the preparation method of intermediate 2 is: S1, adding p-perfluorononenyloxybenzenesulfonyl chloride to acetonitrile solvent, stirring and dispersing, then adding 3,5-bis-aminomethyl-phenol thereto, stirring and reacting at 80-95° C. for 2-5 hours, after the reaction is completed, adding deionized water thereto, stirring, standing and stratifying, taking the organic layer, distilling under reduced pressure, washing with ethanol, and drying to obtain intermediate 1; S2. Add intermediate 1, allyl chloride and cesium carbonate to acetonitrile solvent, stir and disperse, heat to 70-80°C, react for 5-12 hours. After the reaction, add deionized water, stir, stand and separate, take the organic layer, distill under reduced pressure, wash with deionized water, and dry to obtain intermediate 2.

6. The method for preparing the hydrophobic and breathable fabric according to claim 5, characterized in that: In the S1, the molar ratio of p-perfluorononenyloxybenzenesulfonyl chloride to 3,5-bis-aminomethyl-phenol is 2-2.5:

1.

7. The method for preparing the hydrophobic and breathable fabric according to claim 5, characterized in that: In S2, the molar ratio of intermediate 1, propylene chloride and cesium carbonate is 1:1-1.5:1-1.

5.

8. The method for preparing a hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (1), the preparation method of allyl dodecyl dimethyl ammonium chloride is: adding N, N-dimethyl-N-dodecyl tertiary amine to ether solvent, stirring and dispersing, then adding allyl chloride thereto, stirring and reacting at 25-30° C. for 3-6 hours, and after the reaction is completed, washing with ether and drying to obtain allyl dodecyl dimethyl ammonium chloride.

9. The method for preparing the hydrophobic and breathable fabric according to claim 8, characterized in that: The molar ratio of the N,N-dimethyl-N-dodecyl tertiary amine to propylene chloride is 1:0.8-1.

2.

10. The method for preparing a hydrophobic and breathable fabric according to claim 1, characterized in that: In the step (2), the material of the fabric is one of polyester, spandex, nylon and cotton.

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