Super-hydrophobic and antibacterial wool fabric and preparation method thereof

Abstract

The invention relates to a super-hydrophobic and antibacterial wool fabric and a preparation method thereof. The fabric can be prepared by adopting the following method: firstly, preparing silica sol; secondly, preparing a finishing agent solution containing a pore-forming agent; then, the wool fabric is irradiated by ultraviolet light; thirdly, performing infiltration finishing on the wool fabric in the finishing liquid, and finally performing ultrasonic-assisted drying to obtain the super-hydrophobic and antibacterial wool fabric. The surface of the prepared super-hydrophobic and antibacterial wool fabric contains a low-surface-energy substance silicon element, and the apparent contact angle range of water drops on the wool fabric is 161-164 degrees; the antibacterial rate of the prepared wool fabric on escherichia coli reaches 55.0% or above.

Description

Technical Field

[0001] The invention belongs to the technical field of fabric preparation, and particularly relates to a super-hydrophobic and antibacterial wool fabric and a preparation method thereof. Background Art

[0002] As people's pace of life accelerates, people spend less and less time on clothing care, and the simplification of clothing care has become another basic requirement for choosing clothes. Fabrics with super hydrophobicity, self-cleaning and easy antibacterial properties are favored by consumers.

[0003] Wool fabrics are considered the preferred fabric for high-end clothing. They have excellent warmth retention properties, soft feel, bright colors, and are comfortable to wear. In order to meet people's growing needs, functional wool fabrics have been widely studied. Wool itself has many reactive groups, and some substances can be added to this basis to prepare super-hydrophobic wool fabrics. Wool fabrics are also porous textiles, and human sweat, sebum, and skin epidermal debris can easily be adsorbed on them, cultivating bacteria and microorganisms. Therefore, the development of antibacterial properties of wool fabrics is also one of the trends.

[0004] Literature research shows that the super-hydrophobic and antibacterial properties of wool fabrics have received widespread attention. For example, Chinese invention patent application No. 201910053309.X discloses a super-hydrophobic wool fabric and its preparation method: the wool fabric is immersed in a dopamine aqueous solution containing metal ions at 50°C-70°C, and then 1-10kPa of oxygen is blown into the solution to react for a period of time; the fabric is taken out for washing and drying, and the treated fabric is heated at 0.1kg / cm with a multivalent metal ion solution. 2 -0.5kg / cm 2 The super-hydrophobic wool fabric is obtained after padding treatment under pressure and baking; Chinese invention patent application No. 202110496166.7 discloses an antibacterial finishing process for wool fabric: the wool fabric is placed in an oxidation treatment solution for oxidation treatment, and after primary and secondary reduction treatments, the obtained secondary reduction fabric is placed in an antibacterial treatment solution for treatment to obtain an antibacterial wool fabric. The antibacterial wool fabric and hydrophobic wool fabric prepared by these methods still have many shortcomings, such as: the polymerization reaction process of dopamine aqueous solution used in the first method is too long and cannot be mass-produced; the antibacterial wool fabric of the second method has poor long-lasting antibacterial performance after washing, the antibacterial finishing process is complicated, and the antibacterial finishing cost is high; and the above methods cannot integrate antibacterial performance and super-hydrophobic performance together, and cannot coordinate the multiple properties of wool fabrics. Therefore, it is of great practical significance to improve the super-hydrophobic process and antibacterial process of wool fabrics in the prior art to obtain wool fabrics with high super-hydrophobicity and antibacterial performance and low cost. Summary of the invention

[0005] In view of the above-mentioned drawbacks existing in the prior art, the object of the present invention is to provide a super hydrophobic and antibacterial wool fabric and a preparation method thereof.

[0006] The purpose of the present invention is to provide a super-hydrophobic and antibacterial wool fabric, which has the characteristics of super-hydrophobicity, antibacterial, environmental protection, etc. The fabric can be prepared by the following method: first, preparing silica sol; secondly, preparing a finishing agent solution containing a pore-forming agent; then, irradiating the wool fabric with ultraviolet light; thirdly, infiltrating and finishing the wool fabric in the finishing solution; finally, ultrasonic-assisted drying is performed to obtain the super-hydrophobic and antibacterial wool fabric.

[0007] The object of the present invention is achieved through the following technical solutions:

[0008] A method for preparing a super-hydrophobic and antibacterial wool fabric comprises 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 and 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 mixed solution of deionized water, hydrochloric acid and ethanol is prepared by mixing deionized water, 18% hydrochloric acid and anhydrous ethanol in a volume ratio of (50-70):(10-20):(10-20).

[0011] (2) Preparation of pore-forming agent solution: Dissolve ammonium bicarbonate in tap water to prepare a pore-forming agent solution.

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

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

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

[0015] (4) Pretreatment of wool fabric: irradiate the 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) Wetting finishing: Immerse the wool fabric treated in step (4) in the finishing liquid of step (3) for 10 to 20 minutes.

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

[0019] (6) Ultrasonic-assisted drying: The wool fabric treated in step (5) is taken out and dried in an ultrasonic environment at a drying temperature of 50 to 70° C. for 10 to 20 minutes; then, the ultrasonic drying is turned off, the drying temperature is 100 to 120° C. for 10 to 20 minutes, and a super-hydrophobic and antibacterial wool fabric is obtained.

[0020] Preferably, the sound intensity of the ultrasonic wave is: 100-120W / cm 2 .

[0021] The present invention has the following notable features:

[0022] (1) The inventors of the present application 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 the surface roughness and increase the hydrophobicity of wool fabrics.

[0023] (2) The inventors of the present application unexpectedly discovered that the hydrophobicity of wool fabric can be significantly improved by treating the wool fabric with ultraviolet light.

[0024] (3) The surface of the super-hydrophobic and antibacterial wool fabric prepared by the present invention contains silicon element, a low surface energy substance. The apparent contact angle of water droplets on the wool fabric is between 161° and 164°, and it exhibits excellent super-hydrophobicity. After 10 times of washing, the hydrophobicity of the wool fabric is still not significantly weakened. The antibacterial rate of the wool fabric prepared by the present invention against Escherichia coli is more than 55.0%. After 10 times of washing, it still exhibits certain antibacterial performance against Escherichia coli, and the antibacterial rate is more than 40.0%.

[0025] (4) After 10 times of washing, the super-hydrophobic and antibacterial properties of the super-hydrophobic and antibacterial wool fabric prepared by the present invention are not significantly weakened, which indicates that the low surface energy substance silicon element can firmly adhere to the surface of the wool fabric.

[0026] (5) The super-hydrophobic and antibacterial wool fabric prepared by the present invention has a wide range of raw material sources, a simple preparation process, and has a good market promotion prospect. DETAILED DESCRIPTION

[0027] The following examples and comparative examples illustrate the present invention in detail.

[0028] Example 1

[0029] In this embodiment, a method for preparing a super hydrophobic and antibacterial wool fabric comprises the following steps:

[0030] (1) Preparation of silica sol: 100 mL of ethyl 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 at a reaction temperature of 77.5° C. to obtain silica sol.

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

[0032] (3) Preparation of finishing solution: 10 mL of the silica sol prepared in step (1) and 150 mL of the pore-forming agent solution prepared in step (2) were mixed and stirred evenly to prepare a finishing solution.

[0033] (4) Pretreatment of wool fabric: The wool fabric was irradiated with 150 W ultraviolet light for 15 minutes. The ultraviolet light power was 150 W.

[0034] (5) Infiltration finishing: 100 g of the wool fabric treated in step (4) was immersed in 1500 mL of the finishing solution obtained in step (3) for 15 minutes.

[0035] (6) Ultrasonic drying: Take out the wool fabric finished in step (5) and dry it under 110W / cm 2 The fabric was dried in an ultrasonic environment at a temperature of 65°C for 15 minutes. Then, the ultrasonic drying was turned off at a temperature of 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 super hydrophobic and antibacterial wool fabric comprises the following steps:

[0038] (1) Preparation of silica sol: 100 mL of ethyl 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 at a reaction temperature of 70° C. to obtain silica sol.

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

[0040] (3) Preparation of finishing solution: 10 mL of the silica sol prepared in step (1) and 100 mL of the pore-forming agent solution prepared in step (2) were mixed and stirred evenly to prepare a finishing solution.

[0041] (4) Pretreatment of wool fabric: The wool fabric was irradiated with 100 W ultraviolet light for 10 minutes, and the ultraviolet light power was 100 W.

[0042] (5) Infiltration finishing: 100 g of the wool fabric treated in step (4) was immersed in 1000 mL of the finishing solution obtained in step (3) for 10 minutes.

[0043] (6) Ultrasonic drying: Take out the wool fabric treated in step (5) and dry it at 100 W / cm 2 The fabric was dried in an ultrasonic environment at a temperature of 50°C for 10 minutes. Then, the ultrasonic drying was turned off at a temperature of 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 super hydrophobic and antibacterial wool fabric comprises the following steps:

[0046] (1) Preparation of silica sol: 100 mL of ethyl 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 at a reaction temperature of 85° C. to obtain silica sol.

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

[0048] (3) Preparation of finishing liquid: 10 mL of the silica sol prepared in step (1) and 200 mL of the pore-forming agent solution prepared in step (2) were mixed and stirred evenly to prepare a finishing liquid.

[0049] (4) Pretreatment of wool fabric: The wool fabric was irradiated with 200 W ultraviolet light for 20 minutes. The ultraviolet light power was 200 W.

[0050] (5) Infiltration finishing: 100 g of the wool fabric treated in step (4) was immersed in 2000 mL of the finishing solution obtained in step (3) for 20 minutes.

[0051] (6) Ultrasonic drying: Take out the wool fabric finished in step (5) and dry it at 120 W / cm 2The fabric was dried in an ultrasonic environment at a temperature of 70°C for 20 minutes. Then, the ultrasonic drying was turned off at a temperature of 120°C for 20 minutes to obtain a superhydrophobic and antibacterial wool fabric.

[0052] Comparative Example A

[0053] Taking Example 1 as a comparison, in this comparative example, no pore-forming agent is selected, that is, step (2) is not implemented, and the other preparation methods are implemented according to the preparation method of Example 1.

[0054] Comparative Example B

[0055] Taking Example 1 as a comparison, in this comparative example, the wool fabric is not pre-treated, that is, step (4) is not implemented, and the other preparation methods are implemented according to the preparation method of Example 1.

[0056] Comparative Example C

[0057] In contrast to Example 1, in this comparative example, no ultrasound was used, that is, the step (6) of "exposing it to 110W / cm 2 The method of preparing the mixture was as follows: "drying the mixture in an ultrasonic environment at a temperature of 65° C. for 15 minutes" was changed to "drying the mixture at a temperature of 65° C. for 15 minutes", and the other preparation methods were implemented according to the preparation method of Example 1.

[0058] Super hydrophobic performance test:

[0059] In order to better detect the super-hydrophobicity of the super-hydrophobic and antibacterial wool fabric prepared in the present invention, the super-hydrophobic and antibacterial wool fabrics a, b, c, d, e, f prepared in the above-mentioned specific embodiments 1 to 3 and comparative examples A to C of the present invention and the purchased super-hydrophobic wool fabric (purchased from Shanghai Weiren Wool Textile Co., Ltd.) were selected. The apparent contact angle of water droplets on the surface of the super-hydrophobic and antibacterial wool fabric was measured using an XG-CAMA1 basic contact angle tester, and no less than 30 test samples were tested, and the test average value was taken. The fabric to be tested was washed in a standard manner with reference to the washing method of the washing color fastness tester of GB / T 20944.1-2007, and the super-hydrophobic properties of the initial sample and the sample after washing 10 times were tested. The test results are shown in Table 1.

[0060] Table 1 Apparent contact angles of water droplets on wool fabrics a, b, c, d, e, f prepared in Examples 1 to 3 and Comparative Examples A to C and purchased superhydrophobic wool fabrics

[0061]

[0062] As can be seen from Table 1, when the wool fabric is not washed, the apparent contact angle of the water droplets on the wool fabrics a, b, and c prepared in Examples 1 to 3 ranges from 161° to 164°, slightly exceeding the apparent contact angle of the purchased superhydrophobic wool fabric. After 10 times of washing, the hydrophobic properties of fabrics a, b, and c have not weakened. Generally, when the apparent contact angle is greater than 150°, it means that the fabric has superhydrophobicity. It can be considered that the superhydrophobic and antibacterial wool fabric prepared by the present invention has superhydrophobicity. The superhydrophobicity of the superhydrophobic and antibacterial wool fabrics d, e, and f prepared in Comparative Examples AC is significantly poorer, which shows that the pretreatment of the wool fabric, the selection of the pore-forming agent solution, and the drying in an ultrasonic environment all have an important influence on the superhydrophobic properties of the wool fabric.

[0063] Antibacterial performance test:

[0064] The super-hydrophobic and antibacterial wool fabrics a, b, c, d, e, and f prepared in Examples 1-3 and Comparative Examples AC were subjected to antibacterial experiments respectively. The specific antibacterial experimental methods were as follows: the fabrics were qualitatively tested by agar diffusion method according to GB / T 20944.1-2007 "Evaluation of Antibacterial Properties of Textiles Part 1: Agar Plate Diffusion Method", and the fabrics were quantitatively tested for antibacterial properties according to GB / T 20944.3-2008 "Evaluation of Antibacterial Properties of Textiles Part 3: Oscillation Method", and the bacterial species 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 inhibition rates, which were calculated according to 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 fabrics to be tested were subjected to standard washing according to the washing method of the washing color fastness test machine of GB / T20944.1-2007, and the antibacterial properties of the initial samples and the samples after washing 10 times were tested. The test results are shown in Table 2.

[0065] Table 2 Antibacterial rate of super hydrophobic and antibacterial wool fabrics a, b, c, d, e, and f prepared in Examples 1-3 and Comparative Examples 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 can be seen from Table 2, the super-hydrophobic and antibacterial wool fabrics a, b, and c prepared in Examples 1-3 have certain antibacterial properties against Escherichia coli. The antibacterial rate of the super-hydrophobic and antibacterial wool fabrics against Escherichia coli before washing reached more than 55.0%. After 10 washes, the super-hydrophobic and antibacterial wool fabrics still showed certain antibacterial properties against Escherichia coli, with an antibacterial rate of more than 40.0%. The antibacterial rates of the super-hydrophobic and antibacterial wool fabrics d, e, and f prepared in Comparative Examples AC against Escherichia coli were significantly poor, which indicates that the pretreatment of the wool fabric, the selection of the pore-forming agent solution, and the drying in an ultrasonic environment all have an important influence on the super-hydrophobic properties of the wool fabric.

[0068] By studying the antibacterial performance of the superhydrophobic and antibacterial wool fabric prepared by the present invention on Escherichia coli and the apparent contact angle of water droplets on the superhydrophobic and antibacterial wool fabric, it can be considered that the wool fabric prepared by the present invention has the dual functions of superhydrophobicity and antibacterial, among which the superhydrophobicity is obvious and the antibacterial performance needs to be further improved.

Claims

1. A method for preparing super hydrophobic and antibacterial wool fabric, characterized in that: The preparation method comprises 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 and 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: dissolving ammonium bicarbonate in tap water to prepare a pore-forming agent solution; (3) Preparation of finishing liquid: mixing the silica sol prepared in step (1) with the pore-forming agent solution prepared in step (2), and stirring them uniformly to prepare a finishing liquid; (4) Pretreatment of wool fabric: irradiating the wool fabric with ultraviolet light; (5) Wetting finishing: immersing the wool fabric treated in step (4) in the finishing solution of step (3) for 10 to 20 minutes; (6) Ultrasonic-assisted drying: The wool fabric treated in step (5) is taken out and dried in an ultrasonic environment at a drying temperature of 50 to 70° C. for 10 to 20 minutes; then, the ultrasonic drying is turned off, the drying temperature is 100 to 120° C. for 10 to 20 minutes, and a super-hydrophobic and antibacterial wool fabric is obtained.

2. The method for preparing a super-hydrophobic and antibacterial wool fabric according to claim 1, characterized in that: In the step (1), the volume ratio of tetraethyl orthosilicate to anhydrous ethanol is 1:(1-2); the preparation method of 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 super hydrophobic and antibacterial wool fabric according to claim 1, characterized in that: In the step (2), the usage ratio of ammonium bicarbonate to tap water is 1 g: (100-200) mL.

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

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

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

8. A super hydrophobic and antibacterial wool fabric, characterized in that: The invention is prepared by the method according to any one of claims 1 to 7.

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