A superhydrophobic and antibacterial wool fabric and its preparation method

Abstract

This invention relates to a superhydrophobic and antibacterial wool fabric and its preparation method. The fabric can be prepared by the following method: first, preparing a silica sol; second, preparing a finishing agent solution containing a pore-forming agent; then, irradiating the wool fabric with ultraviolet light; third, immersing the wool fabric in the finishing solution; and finally, ultrasonic-assisted drying to obtain the superhydrophobic and antibacterial wool fabric. The surface of the superhydrophobic and antibacterial wool fabric prepared by this invention contains silicon, a low surface energy substance, and the apparent contact angle of water droplets on the wool fabric ranges from 161° to 164°; the wool fabric prepared by this invention achieves an antibacterial rate of over 55.0% against Escherichia coli.

Description

Technical Field

[0001] This invention belongs to the field of fabric preparation technology, specifically relating to a superhydrophobic and antibacterial wool fabric and its preparation method. Background Technology

[0002] With the fast pace of life, people are spending less and less time on clothing care, making simplified clothing care another basic requirement when choosing clothes. Fabrics with superhydrophobic, self-cleaning, and antibacterial properties are highly favored by consumers.

[0003] Wool fabrics are considered the preferred material for high-end clothing due to their excellent warmth retention, soft feel, vibrant colors, and comfortable wear. To meet growing consumer needs, functional wool fabrics have been extensively researched. Wool itself possesses many reactive groups, allowing for the addition of substances to create superhydrophobic wool fabrics. However, wool fabrics are also porous textiles, easily absorbing sweat, sebum, and skin flakes, fostering the growth of bacteria and microorganisms. Therefore, developing antibacterial properties for wool fabrics is also a growing trend.

[0004] Literature review indicates that the superhydrophobic and antibacterial properties of wool fabrics have received widespread attention. For example, Chinese invention patent application number 201910053309.X discloses a superhydrophobic wool fabric and its preparation method: the wool fabric is immersed in a dopamine aqueous solution containing metal ions at 50℃-70℃, followed by the introduction of 1-10 kPa of oxygen into the solution, and the reaction is allowed to proceed for a period of time; the fabric is then removed, washed, and dried, and treated with a polyvalent metal ion solution at 0.1 kg / cm². 2 -0.5kg / cm 2 The superhydrophobic wool fabric is obtained by padding under pressure and baking. Chinese Invention Patent Application No. 202110496166.7 discloses an antibacterial finishing process for wool fabric: the wool fabric is immersed in an oxidation treatment solution for oxidation, followed by one and two reduction treatments. The resulting second-reduced fabric is then immersed in an antibacterial treatment solution to obtain an antibacterial wool fabric. However, these methods still have many shortcomings in preparing antibacterial and hydrophobic wool fabrics. For example, the dopamine aqueous solution polymerization process used in the first method is too time-consuming for large-scale production; the antibacterial wool fabric prepared by the second method has poor long-lasting antibacterial properties after washing, a complex antibacterial finishing process, and high finishing costs; moreover, none of the above methods can integrate antibacterial and superhydrophobic properties, failing to synergistically combine the multiple properties of wool fabric. Therefore, improving the existing superhydrophobic and antibacterial processes for wool fabrics to obtain wool fabrics with high superhydrophobicity and antibacterial properties at a low cost is of significant practical importance. Summary of the Invention

[0005] In view of the above-mentioned drawbacks of the existing technology, the purpose of this invention is to provide a superhydrophobic and antibacterial wool fabric and its preparation method.

[0006] The purpose of this invention is to provide a superhydrophobic and antibacterial wool fabric, which has the characteristics of superhydrophobicity, antibacterial properties, and environmental friendliness. The fabric can be prepared by the following method: First, a silica sol is prepared; second, a finishing agent solution containing a pore-forming agent is prepared; then, the wool fabric is irradiated with ultraviolet light; third, the wool fabric is immersed in the finishing solution for finishing; finally, ultrasonic-assisted drying is performed to obtain the superhydrophobic and antibacterial wool fabric.

[0007] The objective of this invention is achieved through the following technical solution:

[0008] A method for preparing a superhydrophobic and antibacterial wool fabric includes the following steps:

[0009] (1) Preparation of silica sol: Tetraethyl orthosilicate and anhydrous ethanol are mixed and stirred, and then a mixed solution of deionized water, hydrochloric acid and ethanol is added. The mixture is stirred evenly for 1 to 3 hours at a reaction temperature of 70 to 85°C to obtain silica sol.

[0010] Preferably, the volume ratio of tetraethyl orthosilicate to anhydrous ethanol is 1:(1-2), and the method for preparing the mixed solution of deionized water, hydrochloric acid and ethanol is as follows: deionized water, 18% hydrochloric acid by mass fraction and anhydrous ethanol are prepared in a volume ratio of (50-70):(10-20):(10-20).

[0011] (2) Preparation of pore-forming agent solution: Ammonium bicarbonate is dissolved in tap water to prepare pore-forming agent solution.

[0012] Preferably, the ratio of ammonium bicarbonate to tap water is 1g:(100-200)mL.

[0013] (3) Preparation of finishing solution: The silica sol obtained in step (1) is mixed with the pore-forming agent solution obtained in step (2) and stirred evenly to obtain the finishing solution.

[0014] Preferably, the ratio of the amount of silica sol obtained in step (1) to the amount of pore-forming agent solution obtained in step (2) is 1:(10-20).

[0015] (4) Pretreatment of wool fabric: Irradiate wool fabric with ultraviolet light.

[0016] Preferably, the irradiation time is 10 to 20 minutes and the ultraviolet light power is 100 to 200W.

[0017] (5) Immersion finishing: Immerse the wool fabric treated in step (4) into the finishing solution in step (3) for 10 to 20 minutes.

[0018] Preferably, the ratio of the amount of wool fabric treated in step (4) to the amount of finishing solution in step (3) is 1g:(10-20)mL.

[0019] (6) Ultrasonic-assisted drying: Take out the wool fabric processed in step (5) and dry it in an ultrasonic environment at a temperature of 50-70°C for 10-20 minutes; then turn off the ultrasonic drying and dry at a temperature of 100-120°C for 10-20 minutes to obtain a superhydrophobic and antibacterial wool fabric.

[0020] Preferably, the acoustic intensity of the ultrasound is 100–120 W / cm². 2 .

[0021] This invention has the following significant features:

[0022] (1) The inventors of this application have unexpectedly discovered that drying in an ultrasonic environment can significantly improve the surface roughness of wool fabrics; in addition, pore-forming agents can also significantly improve surface roughness and increase the hydrophobicity of wool fabrics.

[0023] (2) The inventors of this application have unexpectedly discovered that treating wool fabric with ultraviolet light can significantly improve the hydrophobicity of wool fabric.

[0024] (3) The surface of the superhydrophobic and antibacterial wool fabric prepared by this invention contains silicon, a low surface energy substance. The apparent contact angle of water droplets on the wool fabric is between 161° and 164°, exhibiting excellent superhydrophobicity. After 10 washes, the hydrophobic properties of the wool fabric are not significantly weakened. The wool fabric prepared by this invention has an antibacterial rate of over 55.0% against Escherichia coli. After 10 washes, it still exhibits certain antibacterial properties against Escherichia coli, with an antibacterial rate of over 40.0%.

[0025] (4) The superhydrophobic and antibacterial wool fabric prepared by the present invention was not significantly weakened after 10 washes, which shows that the low surface energy material silicon element can firmly adhere to the surface of the wool fabric.

[0026] (5) The raw materials for the superhydrophobic and antibacterial wool fabric prepared by this invention are widely available, the preparation process is simple, and it has a good market promotion prospect. Detailed Implementation

[0027] The present invention is described in detail below with reference to the embodiments and comparative examples.

[0028] Example 1

[0029] In this embodiment, a method for preparing a superhydrophobic and antibacterial wool fabric includes the following steps:

[0030] (1) Preparation of silica sol: 100 mL of tetraethyl orthosilicate and 150 mL of anhydrous ethanol were mixed and stirred to obtain solution A; then 60 mL of deionized water, 15 mL of 18% hydrochloric acid and 15 mL of ethanol were mixed to obtain solution B. Solution A was poured into solution B and stirred evenly for 2 hours. The reaction temperature was 77.5℃ to obtain silica sol.

[0031] (2) Preparation of pore-forming agent solution: Dissolve 1g of ammonium bicarbonate in 150mL of tap water to prepare pore-forming agent solution.

[0032] (3) Preparation of finishing solution: Mix 10 mL of silica sol obtained in step (1) with 150 mL of pore-forming agent solution obtained in step (2) and stir evenly to obtain finishing solution.

[0033] (4) Pretreatment of wool fabric: Irradiate the wool fabric with 150W ultraviolet light for 15 minutes.

[0034] (5) Immersion finishing: Select 100g of wool fabric treated in step (4) and immerse it in the finishing solution obtained in step (3) with a volume of 1500mL for 15 minutes.

[0035] (6) Ultrasonic Assisted Drying: Take out the wool fabric processed in step (5) and heat it at 110W / cm². 2 The fabric is dried in an ultrasonic environment at a temperature of 65°C for 15 minutes; then the ultrasonic drying is turned off, and the drying temperature is 110°C for 15 minutes to obtain a superhydrophobic and antibacterial wool fabric.

[0036] Example 2

[0037] In this embodiment, a method for preparing a superhydrophobic and antibacterial wool fabric includes the following steps:

[0038] (1) Preparation of silica sol: 100 mL of tetraethyl orthosilicate and 100 mL of anhydrous ethanol were mixed and stirred to obtain solution A; then 50 mL of deionized water, 10 mL of 18% hydrochloric acid and 10 mL of ethanol were mixed to obtain solution B. Solution A was poured into solution B and stirred evenly for 1 hour. The reaction temperature was 70℃ to obtain silica sol.

[0039] (2) Preparation of pore-forming agent solution: Dissolve 1g of ammonium bicarbonate in 100mL of tap water to prepare pore-forming agent solution.

[0040] (3) Preparation of finishing solution: Mix 10 mL of silica sol obtained in step (1) with 100 mL of pore-forming agent solution obtained in step (2) and stir evenly to obtain finishing solution.

[0041] (4) Pretreatment of wool fabric: Irradiate the wool fabric with 100W ultraviolet light for 10 minutes. The ultraviolet light power is 100W.

[0042] (5) Immersion finishing: Select 100g of wool fabric treated in step (4) and immerse it in the finishing solution obtained in step (3) with a volume of 1000mL for 10 minutes.

[0043] (6) Ultrasonic-assisted drying: Take out the wool fabric processed in step (5) and heat it at 100W / cm². 2 The fabric is dried in an ultrasonic environment at a temperature of 50°C for 10 minutes; then, the ultrasonic drying is turned off, and the drying temperature is set to 100°C for 10 minutes to obtain a superhydrophobic and antibacterial wool fabric.

[0044] Example 3

[0045] In this embodiment, a method for preparing a superhydrophobic and antibacterial wool fabric includes the following steps:

[0046] (1) Preparation of silica sol: 100 mL of tetraethyl orthosilicate and 200 mL of anhydrous ethanol were mixed and stirred to obtain solution A; then 70 mL of deionized water, 70 mL of 18% hydrochloric acid and 70 mL of ethanol were mixed to obtain solution B. Solution A was poured into solution B and stirred evenly for 3 hours. The reaction temperature was 85℃ to obtain silica sol.

[0047] (2) Preparation of pore-forming agent solution: Dissolve 1g of ammonium bicarbonate in 200mL of tap water to prepare pore-forming agent solution.

[0048] (3) Preparation of finishing solution: Mix 10 mL of silica sol obtained in step (1) with 200 mL of pore-forming agent solution obtained in step (2) and stir evenly to obtain finishing solution.

[0049] (4) Pretreatment of wool fabric: Irradiate the wool fabric with 200W ultraviolet light for 20 minutes.

[0050] (5) Immersion finishing: Select 100g of wool fabric treated in step (4) and immerse it in the finishing solution obtained in step (3) with a volume of 2000mL for 20 minutes.

[0051] (6) Ultrasonic Assisted Drying: Take out the wool fabric processed in step (5) and heat it at 120W / cm². 2The wool fabric was dried in an ultrasonic environment at a temperature of 70°C for 20 minutes; then the ultrasonic drying was turned off, and the drying temperature was set to 120°C for 20 minutes to obtain a superhydrophobic and antibacterial wool fabric.

[0052] Comparative Example A

[0053] Compared with Example 1, in this comparative example, no pore-forming agent was selected, that is, step (2) was not implemented, and other preparation methods were implemented according to the preparation method of Example 1.

[0054] Comparative Example B

[0055] Compared with Example 1, in this comparative example, no pretreatment is performed on the wool fabric, that is, step (4) is not implemented, and other preparation methods are implemented according to the preparation method of Example 1.

[0056] Comparative Example C

[0057] Compared with Example 1, in this comparative example, ultrasound is not used, that is: the step (6) of "exposing it to 110W / cm 2 The phrase "drying in an ultrasonic environment at a temperature of 65°C for 15 minutes" should be changed to "drying it at a temperature of 65°C for 15 minutes". Other preparation methods should be carried out according to the preparation method in Example 1.

[0058] Superhydrophobic performance test:

[0059] To better test the superhydrophobicity of the superhydrophobic and antibacterial wool fabrics prepared in this invention, superhydrophobic and antibacterial wool fabrics a, b, c, d, e, and f prepared in the specific embodiments 1-3 and comparative examples A-C of this invention, as well as a purchased superhydrophobic wool fabric (purchased from Shanghai Weiren Wool Textile Co., Ltd.), were selected. The apparent contact angle of water droplets on the surface of the superhydrophobic and antibacterial wool fabrics was measured using an XG-CAMA1 basic contact angle tester. At least 30 samples were tested, and the average value was taken. The fabrics were subjected to standard washing according to the washing method of GB / T 20944.1-2007 (Test for Color Fastness to Wash). The superhydrophobicity of the initial samples and the samples after 10 washes was tested. The test results are shown in Table 1.

[0060] Table 1 shows the apparent contact angles of water droplets on wool fabrics a, b, c, d, e, f prepared in Examples 1-3 and Comparative Examples A-C, and on a purchased superhydrophobic wool fabric.

[0061]

[0062] As shown in Table 1, when the wool fabric is unwashed, the apparent contact angle of water droplets on wool fabrics a, b, and c prepared in Examples 1-3 ranges from 161° to 164°, slightly exceeding the apparent contact angle of the purchased superhydrophobic wool fabric. After 10 washes, the hydrophobic properties of fabrics a, b, and c did not weaken. Generally, when the apparent contact angle is greater than 150°, it indicates that the fabric has superhydrophobicity. Therefore, it can be considered that the superhydrophobic and antibacterial wool fabric prepared in this invention has superhydrophobicity. The superhydrophobic and antibacterial wool fabrics d, e, and f prepared in Comparative Example AC have significantly poorer superhydrophobicity, indicating that the pretreatment of the wool fabric, the selection of the pore-forming agent solution, and drying in an ultrasonic environment all have a significant impact on the superhydrophobic properties of the wool fabric.

[0063] Antibacterial performance test:

[0064] Superhydrophobic and antibacterial wool fabrics (a, b, c, d, e, f) prepared in Examples 1-3 and Comparative Example AC were subjected to antibacterial experiments. The specific antibacterial test methods were as follows: qualitative testing of the fabrics was performed using the agar diffusion method according to GB / T 20944.1-2007 "Evaluation of Antibacterial Properties of Textiles Part 1: Agar Diffusion Method"; quantitative antibacterial properties of the fabrics were determined according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Shaking Method". The bacterial species used were Staphylococcus aureus and Escherichia coli. The qualitative test results of the samples were expressed as inhibition zones, and the quantitative antibacterial activity was expressed as the inhibition rate, calculated using the formula: Inhibition rate = (1-B / A)×100%, where A is the number of viable bacteria on the untreated fabric; B is the number of viable bacteria on the treated fabric. The fabric to be tested was subjected to standard washing according to the washing method of GB / T20944.1-2007 Test Machine for Color Fastness to Wash. The antibacterial properties of the initial sample and the sample after 10 washes were tested. The test results are shown in Table 2.

[0065] Table 2 shows the antibacterial rates of superhydrophobic and antibacterial wool fabrics (a, b, c, d, e, f) prepared in Examples 1-3 and Comparative Example AC against Escherichia coli.

[0066] project a b c d e f Unwashed 55.3％ 56.7％ 55.4％ 23.1％ 28.8％ 21.7％ Wash 10 times 42.5％ 40.7％ 43.6％ 12.6％ 13.8％ 14.5％

[0067] As shown in Table 2, the superhydrophobic and antibacterial wool fabrics a, b, and c prepared in Examples 1-3 exhibit certain antibacterial properties against *Escherichia coli*. Before washing, the superhydrophobic and antibacterial wool fabrics showed an inhibition rate of over 55.0% against *E. coli*. After 10 washes, the superhydrophobic and antibacterial wool fabrics still showed certain antibacterial properties against *E. coli*, with an inhibition rate of over 40.0%. The superhydrophobic and antibacterial wool fabrics d, e, and f prepared in Comparative Example AC showed significantly lower inhibition rates against *E. coli*. This indicates that the pretreatment of the wool fabric, the selection of the pore-forming agent solution, and drying in an ultrasonic environment all have a significant impact on the superhydrophobic properties of the wool fabric.

[0068] By studying the antibacterial properties of the superhydrophobic and antibacterial wool fabric prepared in this invention against Escherichia coli and the apparent contact angle of water droplets on the superhydrophobic and antibacterial wool fabric, it can be concluded that the wool fabric prepared in this invention has dual functions of superhydrophobicity and antibacterial properties. Among them, the superhydrophobicity is obvious, while the antibacterial properties need to be further improved.

Claims

1. A method for preparing a superhydrophobic and antibacterial wool fabric, characterized in that, The preparation method includes the following steps: (1) Preparation of silica sol: Tetraethyl orthosilicate and anhydrous ethanol are mixed and stirred, and then a mixed solution of deionized water, hydrochloric acid and ethanol is added. The mixture is stirred evenly for 1 to 3 hours at a reaction temperature of 70 to 85°C to obtain silica sol. (2) Preparation of pore-forming agent solution: Dissolve ammonium bicarbonate in tap water to prepare pore-forming agent solution; (3) Preparation of finishing solution: The silica sol obtained in step (1) is mixed with the pore-forming agent solution obtained in step (2) and stirred evenly to obtain the finishing solution; (4) Pretreatment of wool fabric: Irradiate wool fabric with ultraviolet light; (5) Immersion finishing: Immerse the wool fabric treated in step (4) into the finishing solution in step (3) for 10 to 20 minutes. (6) Ultrasonic-assisted drying: Take out the wool fabric processed in step (5) and dry it in an ultrasonic environment at a temperature of 50-70°C for 10-20 minutes; then turn off the ultrasonic drying and dry at a temperature of 100-120°C for 10-20 minutes to obtain a superhydrophobic and antibacterial wool fabric.

2. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, In step (1), the volume ratio of tetraethyl orthosilicate to anhydrous ethanol is 1:(1-2); the method for preparing the mixed solution of deionized water, hydrochloric acid and ethanol is as follows: deionized water, 18wt% hydrochloric acid and anhydrous ethanol are prepared in a volume ratio of (50-70):(10-20):(10-20).

3. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, In step (2), the ratio of ammonium bicarbonate to tap water is 1g:(100-200)mL.

4. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, In step (3), the ratio of the amount of silica sol obtained in step (1) to the amount of pore-forming agent solution obtained in step (2) is 1 mL: (10-20) mL.

5. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, In step (4), the irradiation time is 10 to 20 minutes and the ultraviolet light power is 100 to 200W.

6. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, In step (5), the ratio of the amount of wool fabric treated in step (4) to the amount of finishing solution in step (3) is 1g:(10-20)mL.

7. The method for preparing a superhydrophobic and antibacterial wool fabric according to claim 1, characterized in that, The sound intensity of the ultrasound in step (6) is 100-120 W / cm. 2 .

8. A superhydrophobic and antibacterial wool fabric, characterized in that, It is prepared by the method described in any one of claims 1 to 7.

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