阅读说明：本技术 基于多巴胺辅助的巯基-烯点击化学法制备超疏水纺织品 (Preparation of super-hydrophobic textile by dopamine-assisted sulfhydryl-alkene click chemistry method ) 是由 陈国强 王宝亮 于 2021-03-11 设计创作，主要内容包括：本发明公开了一种基于多巴胺辅助的巯基-烯点击化学法制备超疏水纺织品的方法,包括以下步骤：S1.将尼龙56/棉交织织物预处理后,浸泡在多巴胺水溶液中进行改性处理,得到多巴胺改性的尼龙56/棉交织织物；S2.将步骤S1得到的织物浸入含有疏水性硫醇、乙烯基三甲氧基硅烷和光引发剂的混合溶液中,在紫外光的照射下,发生点击偶联反应,从而得到超疏水尼龙56/棉交织织物。通过该法制备的超疏水纺织品,疏水物质是以化学键的形式接枝在织物表面,可以提高超疏水纺织品的耐酸碱、水洗、摩擦、紫外光照等性能。(The invention discloses a method for preparing a super-hydrophobic textile based on a dopamine-assisted sulfhydryl-alkene click chemistry method, which comprises the following steps: s1, pretreating a nylon 56/cotton interwoven fabric, and soaking the nylon 56/cotton interwoven fabric in a dopamine aqueous solution for modification treatment to obtain a dopamine-modified nylon 56/cotton interwoven fabric; s2, soaking the fabric obtained in the step S1 into a mixed solution containing hydrophobic mercaptan, vinyl trimethoxy silane and a photoinitiator, and performing click coupling reaction under the irradiation of ultraviolet light to obtain the super-hydrophobic nylon 56/cotton interwoven fabric. According to the super-hydrophobic textile prepared by the method, the hydrophobic substance is grafted on the surface of the textile in a chemical bond form, so that the performances of acid and alkali resistance, washing, friction, ultraviolet illumination and the like of the super-hydrophobic textile can be improved.)

1. A method for preparing a super-hydrophobic textile based on a dopamine-assisted thiol-ene click chemistry method is characterized by comprising the following steps:

s1, pretreating a nylon 56/cotton interwoven fabric, and soaking the nylon 56/cotton interwoven fabric in a dopamine aqueous solution for modification treatment to obtain a dopamine-modified nylon 56/cotton interwoven fabric;

s2, soaking the fabric obtained in the step S1 into a mixed solution containing hydrophobic mercaptan, vinyl trimethoxy silane and a photoinitiator, and performing click coupling reaction under the irradiation of ultraviolet light to obtain the super-hydrophobic nylon 56/cotton interwoven fabric.

2. The method for preparing a superhydrophobic textile according to the dopamine-assisted thiol-ene click chemistry-based method, as claimed in claim 1, wherein in step S1, the nylon 56/cotton interwoven fabric is an interwoven fabric comprising 50% cotton fibers and 50% nylon fibers.

3. The method for preparing the superhydrophobic textile based on the dopamine-assisted thiol-ene click chemistry method according to claim 1, wherein in step S1, the pretreatment is: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15-30min in each solvent, taking out a cloth sample after cleaning, and drying.

4. The method for preparing a superhydrophobic textile according to claim 1, wherein in step S1, the concentration of the dopamine aqueous solution is 0.5-5g/L, and the pH value is 8.5.

5. The method for preparing the superhydrophobic textile based on the dopamine-assisted thiol-ene click chemistry method according to claim 1, wherein in step S1, the modification treatment conditions are as follows: oscillating for 16-24h at 30-45 ℃.

6. The method for preparing the superhydrophobic textile based on the dopamine-assisted thiol-ene click chemistry method according to claim 1, wherein in step S1, after the modification treatment, the fabric is ultrasonically shaken with absolute ethanol and dried at 45-60 ℃ for 0.5-1 hour.

7. The method for preparing a superhydrophobic textile based on the dopamine-assisted thiol-ene click chemistry method of claim 1, wherein the mixed solution is an ethyl acetate solution containing octadecyl mercaptan, vinyltrimethoxysilane and 2, 2-dimethoxy-2-phenylacetophenone in step S2.

8. The method for preparing the superhydrophobic textile based on the dopamine-assisted thiol-ene click chemistry method according to claim 1, wherein in step S2, the irradiation time of the ultraviolet light is 0.5-1 h.

9. The method for preparing the superhydrophobic textile according to the dopamine-assisted thiol-ene click chemistry method, according to claim 1, wherein in step S2, after the reaction is completed, the fabric is washed with absolute ethanol to remove the residual reactant, and dried at 60-80 ℃ for 1-2 hours.

10. A superhydrophobic textile prepared according to the method of any of claims 1-9.

Technical Field

The invention relates to the technical field of textiles, in particular to a super-hydrophobic textile prepared by a dopamine-assisted sulfydryl-alkene click chemistry method.

Background

Cotton fiber is the most abundant plant fiber, it is cheap, it has excellent comfortableness, reproducibility and biodegradability, the main composition substance is cellulose, because the surface of the cellulose substrate contains abundant hydroxyl, they can absorb moisture and become wet and the durability is poor, therefore we need to endow the super hydrophobic property on the surface of the cotton fiber. Polyamide 56, commonly known as nylon 56, is one of the most popular synthetic fibers, and nylon 56 has a wide range of applications due to its excellent durability, wear resistance and corrosion resistance. The construction of the micro-nano coarse structure on the nylon 56 fiber endows the fiber with super-hydrophobic performance, and can widen the application field of the fiber.

The super-hydrophobic surface generally refers to a surface with a static water contact angle of more than 150 degrees and a sliding angle of less than 10 degrees, and due to the unique wettability, the scientific community digs out the potential application of the super-hydrophobic surface and applies the super-hydrophobic surface to the aspects of self-cleaning, oil-water separation, antifouling and antiscale, micro-fluid transportation and the like. The preparation of the super-hydrophobic surface has two key points, the construction of micro-nano roughness and the use of low surface energy substances. The scientists inspired by them developed many methods for preparing superhydrophobic surfaces, such as nanoparticle loading, layer-by-layer assembly, chemical vapor deposition, etc. By these methods, research institutions have succeeded in imparting superhydrophobic surfaces on different substrates to meet a wide variety of complex and varied requirements. Unfortunately, some super-hydrophobic surfaces are fragile, unstable, and easily affected by external environment, so that the super-hydrophobic performance is lost, and the manufacturing process has the defects of high cost, environmental pollution, long time consumption and the like.

Disclosure of Invention

The invention aims to solve the technical problem of providing a method for preparing a super-hydrophobic textile based on a dopamine-assisted mercapto-alkene click chemistry method.

In order to solve the technical problems, the invention provides the following technical scheme:

the invention provides a method for preparing a super-hydrophobic textile based on a dopamine-assisted mercapto-alkene click chemistry method, which comprises the following steps:

s1, pretreating a nylon 56/cotton interwoven fabric, and soaking the nylon 56/cotton interwoven fabric in a dopamine aqueous solution for modification treatment to obtain a dopamine-modified nylon 56/cotton interwoven fabric;

s2, soaking the fabric obtained in the step S1 into a mixed solution containing hydrophobic mercaptan, vinyl trimethoxy silane and a photoinitiator, and performing click coupling reaction under the irradiation of ultraviolet light to obtain the super-hydrophobic nylon 56/cotton interwoven fabric.

According to the invention, based on the assistance of dopamine, a secondary reaction platform rich in hydroxyl is built on the surfaces of nylon 56 fibers and cotton fibers, then octadecyl mercaptan and vinyl trimethoxy silane (VTMS) are used for click coupling to prepare a super-hydrophobic reagent, and the super-hydrophobic reagent is grafted on a polydopamine aggregate, so that the super-hydrophobic nylon 56/cotton interwoven fabric is successfully prepared, and the static contact angle can reach 161 degrees and the sliding angle can reach 8 degrees. Importantly, the prepared super-hydrophobic fabric can resist corrosive liquid, washing, ultraviolet radiation and mechanical abrasion, has excellent super-hydrophobic stability, and has the functions of self-cleaning and oil-water separation.

Further, in step S1, the nylon 56/cotton interwoven fabric is an interwoven fabric comprising 50% cotton fibers and 50% nylon fibers.

Further, in step S1, the preprocessing is: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15-30min in each solvent, taking out a cloth sample after cleaning, and drying.

Further, in step S1, the concentration of the dopamine aqueous solution is 0.5-5g/L, and the pH value is 8.5.

Further, in step S1, the conditions of the modification process are: oscillating for 16-24h at 30-45 ℃.

Further, in step S1, after the modification treatment, the fabric is ultrasonically shaken with absolute ethyl alcohol and dried at 45 to 60 ℃ for 0.5 to 1 hour.

Further, in step S2, the mixed solution is an ethyl acetate solution containing octadecyl mercaptan, vinyltrimethoxysilane, and 2, 2-dimethoxy-2-phenylacetophenone.

Further, in step S2, the irradiation time of the ultraviolet light is 0.5 to 1 hour.

Further, in step S2, after the reaction is completed, the fabric is washed with anhydrous ethanol to remove the residual reactant, and dried at 60 to 80 ℃ for 1 to 2 hours.

The invention also provides a super-hydrophobic textile prepared by the method.

The invention has the beneficial effects that:

after the nylon 56/cotton interwoven fabric is subjected to super-hydrophobic finishing by adopting the process disclosed by the invention, the roughness of the nylon fibers and the cotton fibers is improved, the surface energy of the interwoven fabric is reduced by the adhesion of hydrophobic substances, and the super-hydrophobic performance is endowed to the interwoven fabric. The results of various performance tests show that: the hydrophobic property is reduced along with the increase of the rubbing times, the ultraviolet illumination time and the washing time of the fabric; the acid and alkali treatment has certain influence on the super-hydrophobic property of the nylon 56/cotton interwoven fabric, but still has better hydrophobic property.

Drawings

FIG. 1 is a schematic representation of a nylon 56/cotton interwoven fabric being superhydrophobic.

FIG. 2 is a side view of the static contact angles of the superhydrophobic fabrics of examples 1-4: a is the static contact angle of example 1; b is the static contact angle of example 2; c is the static contact angle of example 3; d is the static contact angle of example 4.

FIG. 3 is a side view of the surface of the original cotton fiber by electron microscope scanning.

FIG. 4 is a side view of the surface of the virgin nylon fiber by scanning electron microscope.

FIG. 5 is a side view of the surface of the cotton fiber of example 3 taken by electron microscope scanning.

FIG. 6 is a side view of the nylon fiber of example 3 on the surface by scanning electron microscope.

Detailed Description

The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.

Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.

In the following examples and comparative examples, the experimental methods used were conventional unless otherwise specified, and the materials, reagents and the like used were commercially available without otherwise specified.

Example 1

Step 1: pretreatment of nylon 56/cotton interwoven fabric: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15min in each solvent, taking out a cloth sample after cleaning, and drying.

Step 2: modification treatment of nylon 56/cotton interwoven fabric with dopamine: dopamine (0.4g) was dissolved in a conical flask containing deionized water (200 ml), the solubility PH of the liquor was adjusted to 8.5 using Tris and Tris-HCl, and then the raw nylon 56/cotton interwoven fabric (4 cm x 4 cm) was placed in it. The reaction system was sealed in a conical flask and then placed in a low noise shaking and dyeing machine (temperature 45 ℃) for 24 hours. And ultrasonically oscillating the treated fabric with absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 0.5 hour to obtain the dopamine modified nylon 56/cotton interwoven fabric.

And step 3: sulfydryl-alkene click chemical hydrophobization modified nylon 56/cotton interwoven fabric: the dopamine modified nylon 56/cotton interwoven fabric (4 cm x 4 cm) was immersed in a mixed solution containing 100 ml of ethyl acetate and the appropriate ratio of octadecyl mercaptan, vinyltrimethoxysilane and 2, 2-dimethoxy-2-phenylacetophenone, wherein the mass ratio of vinyltrimethoxysilane to octadecyl mercaptan was 2: 1. the reaction system was sealed and irradiated under a UV lamp (250W, λ 365nm) for 0.5 h. After the reaction, the fabric sample was washed with absolute ethanol to remove residual reactants and dried in an oven at 80 ℃ for 1 hour to obtain a superhydrophobic nylon 56/cotton interwoven fabric.

The resulting fabric was tested to have a surface contact angle of 156.

Example 2

Step 1: pretreatment of nylon 56/cotton interwoven fabric: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15min in each solvent, taking out a cloth sample after cleaning, and drying.

Step 2: modification treatment of nylon 56/cotton interwoven fabric with dopamine: dopamine (0.4g) was dissolved in a conical flask containing deionized water (200 ml), the solubility PH of the liquor was adjusted to 8.5 using Tris and Tris-HCl, and then the raw nylon 56/cotton interwoven fabric (4 cm x 4 cm) was placed in it. The reaction system was sealed in a conical flask and then placed in a low noise shaking and dyeing machine (temperature 45 ℃) for 24 hours. And ultrasonically oscillating the treated fabric with absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 0.5 hour to obtain the dopamine modified nylon 56/cotton interwoven fabric.

And step 3: sulfydryl-alkene click chemical hydrophobization modified nylon 56/cotton interwoven fabric: the dopamine modified nylon 56/cotton interwoven fabric (4 cm x 4 cm) was immersed in a mixed solution containing 100 ml of ethyl acetate and the appropriate ratio of octadecyl mercaptan, vinyltrimethoxysilane and 2, 2-dimethoxy-2-phenylacetophenone, wherein the mass ratio of vinyltrimethoxysilane to octadecyl mercaptan was 1: 1. the reaction system was sealed and irradiated under a UV lamp (250W, λ 365nm) for 0.5 h. After the reaction, the fabric sample was washed with absolute ethanol to remove residual reactants and dried in an oven at 80 ℃ for 1 hour to obtain a superhydrophobic nylon 56/cotton interwoven fabric.

The resulting fabric was tested to have a surface contact angle of 152 °.

Example 3

Step 1: pretreatment of nylon 56/cotton interwoven fabric: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15min in each solvent, taking out a cloth sample after cleaning, and drying.

Step 2: modification treatment of nylon 56/cotton interwoven fabric with dopamine: dopamine (0.4g) was dissolved in a conical flask containing deionized water (200 ml), the solubility PH of the liquor was adjusted to 8.5 using Tris and Tris-HCl, and then the raw nylon 56/cotton interwoven fabric (4 cm x 4 cm) was placed in it. The reaction system was sealed in a conical flask and then placed in a low noise shaking and dyeing machine (temperature 45 ℃) for 24 hours. And ultrasonically oscillating the treated fabric with absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 0.5 hour to obtain the dopamine modified nylon 56/cotton interwoven fabric.

And step 3: sulfydryl-alkene click chemical hydrophobization modified nylon 56/cotton interwoven fabric: the dopamine modified nylon 56/cotton interwoven fabric (4 cm x 4 cm) was immersed in a mixed solution containing 100 ml of ethyl acetate and the appropriate ratio of octadecyl mercaptan, vinyltrimethoxysilane and 2, 2-dimethoxy-2-phenylacetophenone, wherein the mass ratio of vinyltrimethoxysilane to octadecyl mercaptan was 1: 2. the reaction system was sealed and irradiated under a UV lamp (250W, λ 365nm) for 0.5 h. After the reaction, the fabric sample was washed with absolute ethanol to remove residual reactants and dried in an oven at 80 ℃ for 1 hour to obtain a superhydrophobic nylon 56/cotton interwoven fabric.

The resulting fabric was tested to have a surface contact angle of 161 °. The contact angles of the fabric after being rubbed 5/10/15/20/25 times with sandpaper loaded with a 100g weight were 153.6 °,154.5 °,154.6 °, 154.4 °, and 152.3 °, respectively. The fabric was placed in solutions with a pH of 1/3/5/7/9/11/13, respectively, and the contact angles after 48h of placement were 152.8 °, 156.1 °, 156.2 °, 161 °, 158.1 °, 154.7 °, 152.4 °, respectively. The fabric is subjected to a Test of the washing fastness of cotton fabrics subjected to click chemical reaction by adopting an SWB-12A type washing fastness tester according to the standard AATCC Test Method 61-2006. After soaping for 45/90/135/180/225/270min, the contact angles were 158.1 °, 158.5 °, 156.5 °, 157 °, 157.7 °, 156.8 °, respectively. After 4/8/12/16h of ultraviolet irradiation, the contact angles of the fabric were 151.9 degrees, 150.9 degrees, 152.3 degrees and 151.2 degrees respectively.

Example 4

Step 1: pretreatment of nylon 56/cotton interwoven fabric: and (3) ultrasonically cleaning the nylon 56/cotton interwoven fabric by using acetone, ethanol and deionized water in sequence for 15min in each solvent, taking out a cloth sample after cleaning, and drying.

Step 2: modification treatment of nylon 56/cotton interwoven fabric with dopamine: dopamine (0.4g) was dissolved in a conical flask containing deionized water (200 ml), the solubility PH of the liquor was adjusted to 8.5 using Tris and Tris-HCl, and then the raw nylon 56/cotton interwoven fabric (4 cm x 4 cm) was placed in it. The reaction system was sealed in a conical flask and then placed in a low noise shaking and dyeing machine (temperature 45 ℃) for 24 hours. And ultrasonically oscillating the treated fabric with absolute ethyl alcohol, and drying the fabric in an oven at 60 ℃ for 0.5 hour to obtain the dopamine modified nylon 56/cotton interwoven fabric.

And step 3: sulfydryl-alkene click chemical hydrophobization modified nylon 56/cotton interwoven fabric: the dopamine modified nylon 56/cotton interwoven fabric (4 cm x 4 cm) was immersed in a mixed solution containing 100 ml of ethyl acetate and the appropriate ratio of octadecyl mercaptan, vinyltrimethoxysilane and 2, 2-dimethoxy-2-phenylacetophenone, wherein the mass ratio of vinyltrimethoxysilane to octadecyl mercaptan was 1: 3. the reaction system was sealed and irradiated under a UV lamp (250W, λ 365nm) for 0.5 h. After the reaction, the fabric sample was washed with absolute ethanol to remove residual reactants and dried in an oven at 80 ℃ for 1 hour to obtain a superhydrophobic nylon 56/cotton interwoven fabric.

The resulting fabric was tested to have a surface contact angle of 155 °.

The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.