Fabric water-repellent finishing agent as well as preparation method and application thereof

Abstract

The invention discloses a fabric water-repellent finishing agent as well as a preparation method and application thereof in the field of fabric finishing agents, and the fabric water-repellent finishing agent is prepared from the following raw materials: polyethylene wax, modified silicon dioxide nano hydrosol, a nonionic surfactant, a silane coupling agent, glacial acetic acid and water. The modified silicon dioxide nano hydrosol is prepared from silicon dioxide nano hydrosol, castor oil, sunflower bud extract and saponin, and a preparation method of the sunflower bud extract comprises the following steps: grinding sunflower bud seedlings, soaking the sunflower bud seedlings in rice vinegar, filtering, extracting filtrate by using ethyl acetate, concentrating, and drying to obtain the sunflower bud extract. And carrying out rotary evaporation treatment on the obtained extraction liquid to obtain the sunflower bud extract. According to the fabric water-repellent finishing agent provided by the invention, a water-repellent layer can be formed on the surface of a fabric which is dried and cured after being soaked by the water-repellent finishing agent, and the water-repellent layer can provide long-acting and stable anti-permeation protection for an inner-layer fabric.

Description

Technical Field

[0001] This invention relates to the field of fabric finishing agents, specifically to a water-repellent finishing agent for fabrics, its preparation method, and its application. Background Technology

[0002] In the textile industry, the water repellency of fabrics is one of the core factors that determine the application scenarios. Improving the water repellency of fabrics can not only directly enhance the fabric's anti-permeability function, but also indirectly improve the fabric's warmth retention and anti-pollution performance. In recent years, with the rise of outdoor activities, research and development on fabric water repellency treatment technology has been gradually expanding.

[0003] Currently, fabric water-repellent finishing technology mainly relies on chemical finishing agents, with mainstream products falling into two main categories: fluorinated and fluorine-free. While fluorinated water-repellent agents achieve excellent water-repellent effects, their production process causes environmental pollution, and they pose significant safety hazards during use, potentially harming human health upon direct skin contact. Fluorine-free water-repellent agents achieve their effect primarily through the compounding of a base material and hydrophobic components; however, existing such agents generally suffer from poor water-repellent durability, making them unsuitable for long-term use. Therefore, this invention provides a fabric water-repellent finishing agent, its preparation method, and its application. Summary of the Invention

[0004] The purpose of this invention is to provide a water-repellent finishing agent for fabrics, its preparation method, and its application in order to solve the above-mentioned problems.

[0005] The present invention achieves the above objectives through the following technical solutions: This invention provides a water-repellent finishing agent for fabrics, the raw materials for which include polyethylene wax, modified silica nano-hydrosol, nonionic surfactant, silane coupling agent, glacial acetic acid, and water. The raw materials for preparing modified silica nano-hydrosol include silica nano-hydrosol, castor oil, sunflower bud extract, and saponins.

[0006] As a further optimization of the present invention, the raw materials for preparing the fabric water-repellent finishing agent, by weight, include 8-12 parts of polyethylene wax, 15-20 parts of modified silica nano-hydrosol, 3-5 parts of nonionic surfactant, 2-4 parts of silane coupling agent, 0.5-1 parts of glacial acetic acid, and 30-40 parts of deionized water.

[0007] As a further optimization of the present invention, the raw materials for preparing the modified silica nano-hydrosol include, by weight, 15-20 parts silica nano-hydrosol, 3-7 parts castor oil, 8-14 parts sunflower bud extract and 1-3 parts saponins.

[0008] The present invention also provides a method for preparing the above-mentioned water-repellent finishing agent for fabrics, specifically including the following steps: (1) The silica nano-hydrosol was subjected to a water bath heating treatment at 40-50℃, and a mixture of castor oil, sunflower bud extract and saponins was added dropwise. After thorough stirring, the modified silica nano-hydrosol was obtained. (2) Mix the nonionic surfactant evenly into deionized water, then slowly add the modified silica nano-hydrosol, and stir thoroughly to obtain a premixed solution; (3) Mix polyethylene wax and silane coupling agent evenly, then add premixed liquid and glacial acetic acid, and then ultrasonically disperse to obtain fabric water-repellent finishing agent.

[0009] As a further optimization of the present invention, in step (1), the sunflower bud extract is prepared by grinding the sunflower buds and soaking them in rice vinegar, filtering them, extracting the filtrate with ethyl acetate, and then rotary evaporating the obtained extract to obtain the sunflower bud extract.

[0010] As a further optimization of the present invention, in step (1), the ultrasonic dispersion process in both steps (1) and (3) is carried out under nitrogen protection.

[0011] As a further optimization of the present invention, in step (3), the ultrasonic dispersion conditions are 60-80℃, 3000-4000rpm, and 20-40min.

[0012] The present invention also provides an application of the above-mentioned water-repellent finishing agent for fabrics, characterized in that the fabric is impregnated with the water-repellent finishing agent and then dried and cured to obtain a functional fabric with surface water repellency.

[0013] As a further optimization of the present invention, the impregnation treatment conditions are 40-60℃, two dips and two rolls, with a roll residue rate of 60%-80%, and the drying and curing conditions are 70-100℃ for 20-40 minutes.

[0014] The beneficial effects of this invention are as follows: The water-repellent finishing agent provided by this invention constructs a stable water-repellent system based on the synergistic effect of modified silica nano-hydrosol and polyethylene wax. After impregnation of fabrics with this water-repellent finishing agent, a continuous water-repellent layer with a micro-rough structure is formed on the fabric surface after drying and curing, achieving the effect of giving the fabric good water repellency. In this water-repellent finishing agent, the treatment method of jointly modifying the modified silica nano-hydrosol with castor oil and sunflower bud extract not only introduces hydrophobic groups to enhance the basic water-repellent properties, but also helps to enhance the antioxidant properties and system homogeneity of the water-repellent finishing agent, thereby enhancing the durability of the water-repellent layer formed on the fabric surface. This allows the water-repellent layer to maintain a good water-repellent protective effect for a long time under repeated washing and long-term light exposure. Detailed Implementation

[0015] The present application will now be described in further detail. It should be noted that the following specific embodiments are only used to further illustrate the present application and should not be construed as limiting the scope of protection of the present application. Those skilled in the art can make some non-essential improvements and adjustments to the present application based on the above application content.

[0016] I. Materials Unless otherwise specified, all methods used in this invention are conventional methods known to those skilled in the art, and all reagents and materials used are commercially available products unless otherwise specified.

[0017] method 1. Preparation of water-repellent finishing agent Example 1 A water-repellent finishing agent for fabrics, the preparation method of which includes the following steps: (1) Preparation of sunflower bud extract: After cleaning and grinding fresh sunflower buds, soak them in rice vinegar at a mass ratio of 1:3 for 5 hours. After filtration, collect the filtrate. Mix the filtrate with ethyl acetate at a volume ratio of 1:2. Extract the filtrate. Then, rotary evaporate the obtained extract (45℃, 0.08MPa) to obtain sunflower bud extract. (2) Take 15 parts by weight of silica nano-hydrosol, 3 parts of castor oil, 8 parts of sunflower bud extract and 1 part of saponin. Under nitrogen protection, heat the silica nano-hydrosol in a water bath at 40°C. Add the mixture of castor oil, sunflower bud extract and saponin to the mixture and stir thoroughly (400 rpm, 5 min) to obtain modified silica nano-hydrosol. (3) By weight, take 8 parts polyethylene wax, 15 parts modified silica nano-hydrosol, 3 parts nonionic surfactant (Tween-80), 2 parts silane coupling agent, 0.5 parts glacial acetic acid and 30 parts deionized water. Mix the nonionic surfactant evenly into the deionized water, and then slowly drop it into the modified silica nano-hydrosol. Stir thoroughly (300 rpm, 8 min) to obtain a premixed solution. (4) Mix polyethylene wax and silane coupling agent evenly, add premixed liquid and glacial acetic acid under nitrogen protection, and then perform ultrasonic dispersion treatment at 60°C, 4000 rpm and 20 min to obtain fabric water repellent finishing agent.

[0018] Example 2 A water-repellent finishing agent for fabrics, the preparation method of which includes the following steps: (1) Preparation of sunflower bud extract: Same as in Example 1; (2) By weight, take 17 parts of silica nano-hydrosol, 5 parts of castor oil, 11 parts of sunflower bud extract and 2 parts of saponins. Under nitrogen protection, heat the silica nano-hydrosol in a water bath at 45°C. Add the mixture of castor oil, sunflower bud extract and saponins to the mixture and stir thoroughly (400 rpm, 5 min) to obtain modified silica nano-hydrosol. (3) By weight, take 11 parts polyethylene wax, 17 parts modified silica nano-hydrosol, 4 parts nonionic surfactant (Tween-80), 3 parts silane coupling agent, 0.6 parts glacial acetic acid and 35 parts deionized water. Mix the nonionic surfactant evenly into the deionized water, and then slowly add the modified silica nano-hydrosol dropwise. Stir thoroughly (300 rpm, 8 min) to obtain a premixed solution. (4) Mix polyethylene wax and silane coupling agent evenly, add premixed liquid and glacial acetic acid under nitrogen protection, and then perform ultrasonic dispersion treatment at 70°C, 3500 rpm and 30 min to obtain fabric water repellent finishing agent.

[0019] Example 3 A water-repellent finishing agent for fabrics, the preparation method of which includes the following steps: (1) Preparation of sunflower bud extract: Same as in Example 1; (2) Take 20 parts by weight of silica nano-hydrosol, 7 parts of castor oil, 14 parts of sunflower bud extract and 3 parts of saponins. Under nitrogen protection, the silica nano-hydrosol is subjected to water bath heating treatment at 50°C. The mixture of castor oil, sunflower bud extract and saponins is added dropwise and stirred thoroughly (400 rpm, 5 min) to obtain modified silica nano-hydrosol. (3) By weight, take 12 parts of polyethylene wax, 20 parts of modified silica nano-hydrosol, 5 parts of nonionic surfactant (Tween-80), 4 parts of silane coupling agent, 1 part of glacial acetic acid and 40 parts of deionized water. Mix the nonionic surfactant evenly into the deionized water, and then slowly drop it into the modified silica nano-hydrosol. Stir thoroughly (300 rpm, 8 min) to obtain a premixed solution. (4) Mix polyethylene wax and silane coupling agent evenly, add premixed liquid and glacial acetic acid under nitrogen protection, and then perform ultrasonic dispersion treatment at 80°C, 3000 rpm and 20 min to obtain fabric water-repellent finishing agent.

[0020] 2. Efficacy testing of water-repellent finishing agents The water-repellent finishing agents obtained in Examples 1-3 were used to impregnate fabric samples (of the same material and size) (50°C, two dips and two nips, 70% pick-up rate). The impregnated samples were then dried (80°C, 30h) to obtain sample fabrics. Untreated fabric samples were used as blank controls. Performance tests were conducted on each group of sample fabrics and blank control fabrics. The test items and methods are as follows: (1) Water repellency test: Fix the fabric 30cm below the spray device and spray it with 250mL of clean water for 1min under the same conditions. Observe the degree of wetting of the fabric after treatment and compare it with the standard water repellency rating card (1-5 levels) for rating: Level 5: No water on the surface, Level 4: Small amount of water on the surface (≤5%), Level 3: Local wetting on the surface (≤20%), Level 2: Significant wetting on the surface (≤50%), Level 1: Most of the surface is wet (>50%). (2) Contact angle test: The contact angle of the water droplet on the sample surface was measured using an OCA 40 contact angle meter. A second test was conducted after the fabric was washed 30 times. The test sites and test conditions were the same for both tests. The water droplet was 10 μL. The reading was taken 1 minute after the water droplet came into contact with the fabric. During the test, 10 sites were selected for each sample to measure the contact angle in sequence. The average value of the 10 contact angle data obtained was taken as the test result of the sample contact angle. (3) Washing resistance test: ① Dry the fabric to constant weight, cool it and weigh it, record it as M0. Then immerse the fabric completely in clean water (25℃), let it stand for 30 minutes and take it out. Hang it for 1 minute to drain the surface water and weigh it again, record it as M1. Water absorption rate (%) = (M1-M0) / M0×100%; ② Wash the fabric 20 times according to the standard machine washing procedure set by AATCC, and dry it after washing; ③ Repeat step ① and test the water absorption rate of the washed fabric. The test results are shown in the table below. As can be seen from the table, compared with the blank control group, the fabric samples treated with the water-repellent finishing agent obtained in Examples 1-3 have a higher water repellency level, a larger surface contact angle, and a lower water absorption rate. This result shows that the water-repellent finishing agent proposed in this invention can significantly improve the surface water repellency of the fabric after being used to impregnate the fabric, thereby reducing the probability of water seepage and absorption.

[0021] ; 3. Detection of factors affecting the efficacy of water-repellent finishing agents (1) Comparative Examples 1 and 2: Based on Example 2, only the components of castor oil and sunflower bud extract in the raw materials for preparing modified silica nano-hydrosol were adjusted (as shown in the table below). ; (2) Comparative Example 3: Based on Example 2, only the preparation method of sunflower bud extract was adjusted. The adjusted preparation method is as follows: after cleaning and grinding fresh sunflower buds, soak them in water at a mass ratio of 1:3 for 5 hours, collect the filtrate after filtration, mix the filtrate with petroleum ether at a volume ratio of 1:2, perform two extraction treatments on the filtrate, and perform rotary evaporation treatment (45°C, 0.08MPa) on the obtained extract to obtain sunflower bud extract; (3) Set up Comparative Example 4: Based on Example 2, only remove the nitrogen protection conditions in steps (2) and (4).

[0022] Fabric samples were treated with the finishing agents obtained in Comparative Examples 1-4 respectively to obtain sample fabrics. The treatment method was the same as in Example 2. Performance tests were conducted on each group of sample fabrics. The test items and methods were the same as in Example 2. Since photoaging is also a key factor affecting fabric performance in daily life, especially for fabrics with protective layers, an additional photoaging test is added to evaluate the impact of different factors on the performance of the water-repellent layer formed by the fabric. The specific testing method for light aging resistance test is as follows: ① Dry the fabric to constant weight, cool it and weigh it, record it as M0, then immerse the fabric completely in clean water (25℃), let it stand for 30 minutes and then take it out, hang it for 1 minute to drain the surface water, weigh it again and record it as M1, water absorption rate (%) = (M1-M0) / M0×100%; ② According to the standard specified by AATCC TM16, the fabric is subjected to 240 hours of outdoor simulated light treatment; ③ Repeat step ① and test the water absorption rate of the fabric after washing.

[0023] The test results are shown in the table below. From the table, we can see that: (1) Compared with Example 2, in Comparative Examples 1 and 2, the water repellency level of the fabric is lower, the surface contact angle is smaller, and the water absorption rate is higher. This result indicates that when castor oil and sunflower bud extract are used together to modify silica water nano-hydrosol, the modified silica water nano-hydrosol can effectively enhance the efficacy of the water repellent finishing agent, that is, enhance the water repellency and anti-penetration effect of the water repellent layer formed on the surface of the fabric treated with the water repellent finishing agent. (2) Compared with Example 2, in Examples 3 and 4, the difference in water absorption rate of the fabric before and after washing and before and after light exposure is increased. Among them, the difference between Comparative Example 4 and Comparative Example 3 is particularly significant. This result indicates that compared with sunflower bud extract obtained by water extraction (Comparative Example 3), the water-repellent finishing agent prepared by sunflower bud extract obtained by vinegar extraction (Example 2) has better durability in the water-repellent layer formed on the fabric surface after being applied to the fabric. In addition, providing nitrogen protection conditions during the preparation of the water-repellent finishing agent can also effectively improve the performance of the water-repellent finishing agent, thereby improving the durability of the water-repellent layer on the fabric surface.

[0024] ; The embodiments described above are merely examples of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the present invention. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these modifications and improvements all fall within the scope of protection of the present invention.

Claims

1. A water-repellent finishing agent for fabrics, characterized in that: The raw materials for preparing the fabric water-repellent finishing agent include polyethylene wax, modified silica nano-hydrosol, nonionic surfactant, silane coupling agent, glacial acetic acid, and water. The raw materials for preparing modified silica nano-hydrosol include silica nano-hydrosol, castor oil, sunflower bud extract, and saponins.

2. The fabric water-repellent finishing agent according to claim 1, characterized in that: The raw materials for preparing the fabric water-repellent finishing agent, by weight, include 8-12 parts polyethylene wax, 15-20 parts modified silica nano-hydrosol, 3-5 parts nonionic surfactant, 2-4 parts silane coupling agent, 0.5-1 parts glacial acetic acid, and 30-40 parts deionized water.

3. The fabric water-repellent finishing agent according to claim 1, characterized in that: The raw materials for preparing modified silica nano-hydrosols, by weight, include 15-20 parts silica nano-hydrosols, 3-7 parts castor oil, 8-14 parts sunflower bud extract, and 1-3 parts saponins.

4. A method for preparing a fabric water-repellent finishing agent as described in any one of claims 1-3, characterized in that: Specifically, the following steps are included: (1) The silica nano-hydrosol was subjected to a water bath heating treatment at 40-50℃, and a mixture of castor oil, sunflower bud extract and saponins was added dropwise. After thorough stirring, the modified silica nano-hydrosol was obtained. (2) Mix the nonionic surfactant evenly into deionized water, then slowly add the modified silica nano-hydrosol, and stir thoroughly to obtain a premixed solution; (3) Mix polyethylene wax and silane coupling agent evenly, then add premixed liquid and glacial acetic acid, and then ultrasonically disperse to obtain fabric water-repellent finishing agent.

5. The preparation method according to claim 4, characterized in that: In step (1), the sunflower bud extract is prepared by grinding sunflower buds and soaking them in rice vinegar, filtering them, extracting the filtrate with ethyl acetate, and then rotary evaporating the obtained extract to obtain sunflower bud extract.

6. The preparation method according to claim 4, characterized in that: In step (1), the ultrasonic dispersion process in both step (1) and step (3) is carried out under nitrogen protection.

7. The preparation method according to claim 4, characterized in that: In step (3), the ultrasonic dispersion conditions are 60-80℃, 3000-4000rpm, and 20-40min.

8. The application of a fabric water-repellent finishing agent as described in any one of claims 1-3, characterized in that, The fabric is impregnated with the aforementioned water-repellent finishing agent, and then the impregnated fabric is dried and cured to obtain a functional fabric with a water-repellent surface.

9. The application according to claim 8, characterized in that: The impregnation treatment conditions are 40-60℃, two dips and two rolls, with a roll-off rate of 60%-80%, and the drying and curing conditions are 70-100℃ for 20-40 minutes.