Durable gallium-iron alloy antibacterial textile fabric and preparation method and application thereof
By loading gallium-iron alloy on textile fabrics, the problems of poor antibacterial effect and insufficient durability of existing antibacterial materials are solved, and high-efficiency, multi-mechanism antibacterial performance and durability are achieved, which is suitable for the field of textile fabrics.
Patent Information
- Application Number
- CN202410945940.1
- Authority / Receiving Office
- CN · China
- Patent Type
- Patents(China)
- Current Assignee / Owner
- Filing Date
- 2024-07-15
- Publication Date
- 2025-10-10
- Estimated Expiration
- 2044-07-15
AI Technical Summary
Existing antibacterial materials have poor antibacterial effects and durability, and are prone to causing pathogen resistance. Traditional metal antibacterial mechanisms are single, resulting in the inability of materials to effectively prevent the spread of pathogens and increasing economic and environmental burdens.
Gallium-iron alloy is used as an antibacterial agent. Gallium and iron are loaded on textile fabrics through plasma cleaning and immersion processes to form a variety of antibacterial particles, enhance the surface roughness and load fastness of the fiber, and the preparation process is green and environmentally friendly.
It achieves high-efficiency antibacterial performance with an inhibition rate of up to 99.99%. It has multiple antibacterial mechanisms, improves wear resistance and water washability, and the preparation process is free of toxic organic solvents, making it environmentally friendly and sustainable.
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Figure CN118745659B_ABST
Abstract
Description
TECHNICAL FIELD
[0001] The application belongs to the field of textile fabrics, and particularly relates to a durable gallium-iron alloy antibacterial textile fabric and a preparation method and application thereof. BACKGROUND
[0002] With the development of human society, bacterial infection has become an important public health problem. The inherent defects of the current antibacterial materials highlight the urgent need for innovation of antibacterial materials. Many existing materials have poor antibacterial effect and cannot effectively prevent the spread of pathogens. In addition, with the development of pathogens, drug resistance is widespread, further weakening the efficacy of antibacterial materials. And the dependence on single antibacterial mechanism, such as traditional antibacterial inorganic metal particles of silver and copper, limits the activity range and produces drug resistance. In addition, most of the current antibacterial materials for protection are disposable, which also exacerbates the limitations of antibacterial materials and increases the economic and environmental burden. Therefore, how to solve the defects of poor antibacterial effect, poor durability, non-reusable caused by traditional antibacterial materials, single metal antibacterial mechanism and easy to cause drug resistance of pathogens is still a difficult problem. SUMMARY
[0003] In view of the deficiencies of the prior art, the application aims to provide a durable gallium-iron alloy antibacterial textile fabric.
[0004] Another object of the application is to provide a preparation method of the durable gallium-iron alloy antibacterial textile fabric.
[0005] The object of the application is achieved by the following technical solutions.
[0006] A durable gallium-iron alloy antibacterial textile fabric comprises a textile fabric and a gallium-iron alloy loaded on the surface of the textile fabric.
[0007] In the above technical solution, the ratio of gallium to iron in the gallium-iron alloy is (1.53-2.03):1 by mass fraction.
[0008] A preparation method of a durable gallium-iron alloy antibacterial textile fabric comprises the following steps:
[0009] 1) The textile fabric is subjected to plasma cleaning for 10-60 min, and then taken out and subjected to multiple immersions in a gallium (Ga) dispersion liquid to obtain a gallium-containing textile fabric, wherein each immersion comprises: immersion in the gallium dispersion liquid for 10-60 min, and then taking out and drying.
[0010] In the step 1), the textile fabric is a desized pure cotton fabric, a non-woven fabric or a desized aramid fabric, and the material of the non-woven fabric includes polypropylene (PP) and polyethylene (PE).
[0011] In the above technical solution, the method for obtaining the desized pure cotton fabric comprises: soaking the pure cotton fabric in an alkaline solution at 80° C. to 90° C. for 0.5 to 1 hour, taking it out, rinsing it with deionized water, and drying it.
[0012] In the above technical solution, the method for obtaining the desized aramid fabric includes: soaking the aramid fabric in an alkaline solution at 80° C. to 90° C. for 0.5 to 1 hour, taking it out, rinsing it with deionized water, and drying it.
[0013] In the above technical solution, the alkaline solution includes sodium hydroxide (NaOH), sodium carbonate (Na2CO3) and water, and the pH of the alkaline solution is 12-13.
[0014] In the above technical solution, the concentration of sodium hydroxide in the alkaline solution is 1-1.5 wt %, and the concentration of sodium carbonate in the alkaline solution is 0.5-1 wt %.
[0015] In the above technical solution, the non-woven fabric is obtained by melt-blowing the raw materials after melting and granulating, wherein the raw materials are polypropylene (PP) and polyethylene (PE).
[0016] In step 1), one or both sides of the textile fabric are plasma cleaned.
[0017] In the step 1), the gallium dispersion is a mixture of metallic gallium and anhydrous ethanol, and the concentration of gallium in the gallium dispersion is 0.5-1 wt%.
[0018] In step 1), the drying is vacuum drying or hair dryer drying, the vacuum drying temperature is 80-90°C, the vacuum drying time is 40-60 minutes, the hair dryer drying conditions are a wind speed of 5-8 m / s, and the hair dryer drying temperature is 40-60°C.
[0019] In the step 1), the plasma cleaning is performed in a mixed gas atmosphere of nitrogen and oxygen, with the volume ratio of nitrogen to oxygen being (6-8):(2-4).
[0020] In the step 1), plasma cleaning is performed under irradiation with ultraviolet light in the UVC band, wherein the wavelength of the ultraviolet light in the UVC band is 250 to 260 nm.
[0021] In the step 1), the temperature of the plasma cleaning is 30-50° C., the frequency of the plasma cleaning is 12-14 MHz, and the power of the plasma cleaning is 450-550 W.
[0022] In the step 1), the soaking is performed 1 to 5 times.
[0023] 2) Soaking the gallium-containing textile fabric in a ferrous sulfate (FeSO4) solution for 3 to 5 hours, taking it out, and drying it to obtain a durable gallium-iron alloy antibacterial textile fabric.
[0024] In the step 2), the drying temperature is 60-80° C., and the drying time is at least 30 minutes.
[0025] In step 2), the ferrous sulfate (FeSO4) solution includes: a mixture of ferrous sulfate (FeSO4), an antioxidant and water, the concentration of ferrous sulfate (FeSO4) in the ferrous sulfate (FeSO4) solution is 0.5-0.55 mol / L, and the concentration of the antioxidant in the ferrous sulfate (FeSO4) solution is 1-2 g / L.
[0026] In the above technical solution, the antioxidant is ascorbic acid (AA).
[0027] The use of the durable gallium-iron alloy antibacterial textile fabric in the preparation of antibacterial materials.
[0028] Compared with the prior art, the present invention has the following beneficial effects:
[0029] (1) Durable gallium-iron alloy antibacterial textile fabrics have excellent antibacterial properties, with an inhibition rate of up to 99.99% against Staphylococcus aureus.
[0030] (2) Gallium and iron can undergo a substitution reaction, resulting in a variety of antibacterial particles on the surface, enriching the antibacterial mechanism.
[0031] (3) After plasma cleaning, the fiber surface becomes rough and the load fastness increases, making it have excellent wear resistance and water washability.
[0032] (4) Through the electrical substitution reaction, the load becomes more solid.
[0033] (5) No toxic organic solvents are used in the preparation process, the preparation method is simple, the reaction conditions are mild, and it is green and environmentally friendly. BRIEF DESCRIPTION OF THE DRAWINGS
[0034] Figure 1 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial cotton fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ SEM images of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8;
[0035] Figure 2 EDS characterization of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5;
[0036] Figure 3 (a) is a quality bar graph of the first non-woven fabric, the gallium-containing non-woven fabric, and the durable gallium-iron alloy antibacterial textile fabric; Figure 3 (b) is Figure 3 (a) Fitting curve of the mass of Fe and the mass of Ga in the prepared durable gallium-iron alloy antibacterial textile fabric;
[0037] Figure 4 (a) is the original mass of the first non-woven fabric and the gallium-containing non-woven fabric and the remaining mass after 20 draggings, Figure 4 (b) is the original mass of the first non-woven fabric and the gallium-containing non-woven fabric and the remaining mass after 40 dragging. Figure 4 (c) is the original mass of the first non-woven fabric and the gallium-containing non-woven fabric and the remaining mass after 60 dragging. Figure 4 (d) is the original mass of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric and the remaining mass after 20 draggings, Figure 4 (e) is the original mass of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric and the remaining mass after 40 dragging, Figure 4 (f) is the original mass of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric and the remaining mass after being dragged 60 times;
[0038] Figure 5 This is the XPS characterization of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5, where (a) is the C1s spectrum, (b) is the O1s spectrum, (c) is the Ga3d spectrum, and (d) is the Fe2p spectrum;
[0039] Figure 6 (a) is the Fe-containing 2+ TG test results of the antibacterial PP / PE nonwoven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5, (b) the antibacterial PP / PE nonwoven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE nonwoven fabric containing Fe prepared in Example 4 2+ DSC test results of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5;
[0040] Figure 7 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial cotton fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ Breathability of the antibacterial PP / PE nonwoven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6;
[0041] Figure 8 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial cotton fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ Moisture permeability of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6;
[0042] Figure 9 The water contact angle histograms of the first non-woven fabric, the gallium-containing non-woven fabric, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5;
[0043] Figure 10 The average antibacterial rates of the antibacterial pure cotton fabric containing Ga prepared in Example 1 and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 and 6 against Escherichia coli and Staphylococcus aureus;
[0044] Figure 11 The antibacterial effect diagram shows the maximum antibacterial rate against Escherichia coli and Staphylococcus aureus;
[0045] Figure 12 The average antibacterial rate of the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 7 to 8 against Escherichia coli and Staphylococcus aureus;
[0046] Figure 13 This is a diagram showing the inhibition zone effect of the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 and 6 on Staphylococcus aureus;
[0047] Figure 14 This is a bar graph showing the average antibacterial rates of the antibacterial pure cotton fabric containing Ga prepared in Example 1 and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8 against Escherichia coli and Staphylococcus aureus;
[0048] Figure 15 (a) and (b) are control groups of Escherichia coli and Staphylococcus aureus, respectively. (c) and (d) are antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 after 50 washes on the two bacteria. (e) and (f) are antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 after 50 washes on the two bacteria.
[0049] Figure 16 (a) and (b) are graphs showing the antibacterial effect of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 7 on two types of bacteria after 50 washes; (c) and (d) are graphs showing the antibacterial effect of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 8 on two types of bacteria after 50 washes;
[0050] Figure 17 This is a bar graph showing the antibacterial rates of the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8 against Escherichia coli and Staphylococcus aureus after 50 washes;
[0051] Figure 18 These are the wear resistance test results of the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 and 6. DETAILED DESCRIPTION
[0052] The technical solution of the present invention is described in detail below with reference to the embodiments and drawings.
[0053] The purchase sources and processing methods of the raw materials involved in the following examples are as follows:
[0054] Pure cotton fabric was purchased from Zhengzhou Simian Textile Co., Ltd. (Zhengzhou, China). The method for obtaining desized pure cotton fabric includes: soaking the pure cotton fabric in an alkaline solution at 80°C for 1 hour, taking it out, rinsing it with deionized water, and vacuum drying it at 80°C for 60 minutes, wherein the alkaline solution includes: sodium hydroxide (NaOH), sodium carbonate (Na2CO3) and water, the concentration of NaOH in the alkaline solution is 1wt%, the concentration of Na2CO3 in the alkaline solution is 0.5wt%, and the pH of the alkaline solution is 13. The desized pure cotton fabric is a plain weave with a size of 0.04m 2 , thickness is 0.16mm.
[0055] The non-woven fabric was obtained by melt-blowing the raw materials after melt granulation. The raw materials were polypropylene (PP) and polyethylene (PE). The ratio of polypropylene (PP) to polyethylene (PE) was 90:10 by mass. Polypropylene (PP) and polyethylene (PE) were purchased from Suzhou Tumei Plastics Import and Export Co., Ltd. (Suzhou, China). The size of the non-woven fabric was 0.04m 2 , thickness is 0.22mm.
[0056] Aramid 1414 plain weave fabric and aramid 1313 plain weave fabric were purchased from Yixing Carbon Technology Co., Ltd., China. The method for obtaining desized aramid 1414 plain weave fabric and desized aramid 1313 plain weave fabric includes: boiling the aramid 1414 plain weave fabric and the aramid 1313 plain weave fabric in an alkaline solution at 90°C for 1 hour, taking out, rinsing with deionized water, and drying with a hair dryer at 50°C for 40 minutes, wherein the alkaline solution includes: sodium hydroxide (NaOH), sodium carbonate (Na2CO3) and water, the concentration of NaOH in the alkaline solution is 1wt%, the concentration of Na2CO3 in the alkaline solution is 0.5wt%, and the pH of the alkaline solution is 13. The size of the desized aramid 1414 plain weave fabric is 0.04m 2 , thickness is 0.30mm; desized aramid 1313 plain weave fabric size is 0.04m 2, thickness is 0.40mm.
[0057] The gallium dispersion is a mixture of metallic gallium and anhydrous ethanol, with a gallium concentration of 1 wt %. The preparation process for the gallium dispersion is to place 1 g of metallic gallium in 99 g of anhydrous ethanol and then ultrasonicate for 30 minutes at an ultrasonic power of 80 W to obtain the gallium dispersion.
[0058] The ferrous sulfate (FeSO4) solution comprises a mixture of ferrous sulfate (FeSO4), an antioxidant, and water. The concentration of ferrous sulfate (FeSO4) in the ferrous sulfate (FeSO4) solution is 0.5 mol / L, and the concentration of the antioxidant in the ferrous sulfate (FeSO4) solution is 1.5 g / L. The antioxidant is ascorbic acid (AA). Ferrous sulfate is ferrous sulfate heptahydrate, purchased from Tianjin Fengchuan Chemical Reagent Technology Co., Ltd. Gallium (Ga), sodium hydroxide (NaOH), and sodium carbonate (Na2CO3) were purchased from Shanghai MacLean Biochemical Technology Co., Ltd.
[0059] Anhydrous ethanol (alcohol) was purchased from Tianjin Jiangtian Chemical Technology Co., Ltd.;
[0060] All chemicals and solvents were of analytical grade and required no further purification;
[0061] Deionized water was used for all water;
[0062] Soybean peptone and agar powder were purchased from Beijing Solebow Technology Co., Ltd.;
[0063] PBS buffer, Gram-negative Escherichia coli (ATCC-25922) and Gram-positive Staphylococcus aureus (ATCC-25923) were purchased from Aoboxing Biotechnology Co., Ltd.
[0064] Models of the instruments involved in the following embodiments:
[0065] Electronic balance, model: ES / EX1055B, source: Tianjin Deant Sensing Technology Co., Ltd.;
[0066] Vacuum drying oven, model: 101-4, source: Taizhou Mengyi Automatic Control Equipment Co., Ltd.
[0067] Thermogravimetric analyzer, model: TG 209F3, source: NETZSCH, Germany;
[0068] Differential scanning calorimeter, model: 209F3, source: NETZSCH, Germany;
[0069] Desktop scanning electron microscope, model: Phenom XL, source: Phenom-World, Netherlands;
[0070] X-ray photoelectron spectrometer, model: Thermo Fisher, source: NEXSA, USA;
[0071] Fabric air permeability tester, model: FX3300-IV, source: TEXTEST, Switzerland;
[0072] Fabric moisture permeability tester, model: YG601E-Ⅱ, source: Wenzhou Baien Instrument Co., Ltd.
[0073] Washing color fastness tester, model: SW-10, source: Laizhou Electronic Instrument Co., Ltd.
[0074] Martindale abrasion tester, model: YG401E-4, source: Quanzhou Meibang Instrument Co., Ltd.
[0075] In the following embodiments, the wavelength of ultraviolet light in the UVC band is 253 to 260 nm.
[0076] In the following embodiments, the frequency of plasma cleaning is 13 MHz, and the power of plasma cleaning is 500 W.
[0077] Example 1
[0078] A method for preparing antibacterial pure cotton fabric containing Ga comprises the following steps:
[0079] In a mixed gas atmosphere of nitrogen and oxygen (the volume ratio of nitrogen and oxygen is 7:3), both sides of the desized pure cotton fabric were plasma cleaned at 40°C for 30 minutes (plasma cleaning was carried out under ultraviolet light in the UVC band). After plasma cleaning, the fabric was taken out and immersed in a gallium dispersion for 5 times to obtain an antibacterial pure cotton fabric containing Ga, wherein each immersion included: immersing in the gallium dispersion for 60 minutes, taking out, and drying with a hair dryer at 50°C for 40 minutes.
[0080] Example 2
[0081] A method for preparing an antibacterial PP / PE non-woven fabric containing Ga comprises the following steps:
[0082] In a mixed gas atmosphere of nitrogen and oxygen (the volume ratio of nitrogen and oxygen is 7:3), both sides of the non-woven fabric were plasma cleaned at 40°C for 30 minutes (plasma cleaning was carried out under ultraviolet light in the UVC band). After plasma cleaning, the non-woven fabric was taken out and immersed in a gallium dispersion for 5 times to obtain an antibacterial PP / PE non-woven fabric containing Ga, wherein each immersion included: immersing in the gallium dispersion for 60 minutes, taking out, and drying with a hair dryer at 40°C for 40 minutes.
[0083] Example 3
[0084] A type containing Fe 2+ The preparation method of antibacterial pure cotton fabric comprises the following steps:
[0085] In a mixed gas atmosphere of nitrogen and oxygen (the volume ratio of nitrogen and oxygen is 7:3), both sides of the desized pure cotton fabric were plasma cleaned at 40℃ for 30min (plasma cleaning was carried out under ultraviolet light in the UVC band). After plasma cleaning, the fabric was taken out and immersed in ferrous sulfate (FeSO4) solution for 5h, taken out, and vacuum dried at 60℃ for 30min to obtain FeSO4. 2+ Antibacterial cotton fabric.
[0086] Example 4
[0087] A type containing Fe 2+ The preparation method of antibacterial PP / PE non-woven fabric comprises the following steps:
[0088] In a mixed gas atmosphere of nitrogen and oxygen (the volume ratio of nitrogen and oxygen is 7:3), both sides of the non-woven fabric were plasma cleaned at 40 ° C for 30 minutes (plasma cleaning was carried out under ultraviolet light in the UVC band), taken out after plasma cleaning, immersed in ferrous sulfate (FeSO4) solution for 5 hours, taken out, and vacuum dried at 80 ° C for 30 minutes to obtain Fe 2+ Antibacterial PP / PE non-woven fabric.
[0089] Example 5
[0090] A method for preparing a durable gallium-iron alloy antibacterial textile fabric comprises the following steps:
[0091] 1) In a mixed gas atmosphere of nitrogen and oxygen (nitrogen to oxygen volume ratio of 7:3), both sides of the non-woven fabric were plasma cleaned at 40°C for 30 minutes (the plasma cleaning was performed under ultraviolet light in the UVC band), then removed from the non-woven fabric after plasma cleaning and immersed in a gallium dispersion five times to obtain a gallium-containing textile fabric, wherein each immersion comprised: immersing in the gallium dispersion for 60 minutes, removing from the non-woven fabric, and drying with a hair dryer at 40°C for 40 minutes.
[0092] 2) The gallium-containing textile fabric was immersed in a ferrous sulfate (FeSO4) solution for 5 hours, taken out, and vacuum-dried at 80°C for 30 minutes to obtain a durable gallium-iron alloy antibacterial textile fabric.
[0093] Example 6
[0094] A method for preparing a durable gallium-iron alloy antibacterial textile fabric comprises the following steps:
[0095] 1) In a mixed gas atmosphere of nitrogen and oxygen (nitrogen to oxygen volume ratio of 7:3), both sides of a desized pure cotton fabric were plasma cleaned at 40°C for 30 min (plasma cleaning was performed under ultraviolet light in the UVC band). After plasma cleaning, the fabric was taken out and immersed in a gallium dispersion five times to obtain a gallium-containing textile fabric, wherein each immersion comprised: immersing in the gallium dispersion for 10 min, and taking out and drying, wherein the drying was performed by a hair dryer, and the hair dryer drying conditions were a wind speed of 5 m / s and a drying temperature of 40°C.
[0096] 2) The gallium-containing textile fabric was immersed in a ferrous sulfate (FeSO4) solution for 5 hours, taken out, and vacuum-dried at 80°C for 30 minutes to obtain a durable gallium-iron alloy antibacterial textile fabric.
[0097] Example 7
[0098] A method for preparing a durable gallium-iron alloy antibacterial textile fabric comprises the following steps:
[0099] 1) In a mixed gas atmosphere of nitrogen and oxygen (nitrogen to oxygen volume ratio of 7:3), both sides of a desized aramid fabric (desized aramid 1414 plain weave fabric) were plasma cleaned at 40°C for 60 min (plasma cleaning was performed under UVC band ultraviolet light irradiation). After plasma cleaning, the fabric was taken out and immersed in a gallium dispersion five times to obtain a gallium-containing textile fabric, wherein each immersion comprised: immersing in the gallium dispersion for 10 min, and then taking out and drying, wherein the drying was performed by a hair dryer, and the hair dryer drying conditions were a wind speed of 5 m / s and a drying temperature of 40°C.
[0100] 2) The gallium-containing textile fabric was immersed in a ferrous sulfate (FeSO4) solution for 5 hours, taken out, and vacuum-dried at 80°C for 30 minutes to obtain a durable gallium-iron alloy antibacterial textile fabric.
[0101] Example 8
[0102] A method for preparing a durable gallium-iron alloy antibacterial textile fabric comprises the following steps:
[0103] 1) In a mixed gas atmosphere of nitrogen and oxygen (nitrogen to oxygen volume ratio of 7:3), both sides of a desized aramid fabric (desized aramid 1313 plain weave fabric) were plasma cleaned at 40°C for 60 min (plasma cleaning was performed under ultraviolet light). After plasma cleaning, the fabric was taken out and immersed in a gallium dispersion five times to obtain a gallium-containing textile fabric, wherein each immersion comprised: immersing in the gallium dispersion for 20 min, and then taking out and drying, wherein the drying was performed using a hair dryer, and the hair dryer drying conditions were a wind speed of 5 m / s and a drying temperature of 60°C.
[0104] 2) The gallium-containing textile fabric was immersed in a ferrous sulfate (FeSO4) solution for 5 hours, taken out, and vacuum-dried at 80°C for 60 minutes to obtain a durable gallium-iron alloy antibacterial textile fabric.
[0105] Figure 1 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial cotton fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ SEM images of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8.
[0106] The Ga dispersion (gallium dispersion) was characterized and it was found that Ga in the Ga dispersion was in the form of round spheres. The SEM of Example 1 showed that there were round spheres of Ga on the fiber surface of the Ga-containing antibacterial pure cotton fabric; the SEM of Example 2 showed that there were round spheres of Ga on the fiber surface of the Ga-containing antibacterial PP / PE non-woven fabric, which showed that Ga was successfully loaded. The SEM of Examples 3-4 showed that the Ga-containing Fe 2+ There is no significant difference between the surface of antibacterial cotton fabric and antibacterial PP / PE non-woven fabric. The SEM of Example 5 shows that the surface of the durable gallium-iron alloy antibacterial textile fabric has obvious irregular gallium-iron alloy loading, which is specifically manifested as the presence of blocky substances around the gallium spheres. It is further characterized by energy dispersive X-ray spectroscopy (EDS) ( Figure 2 ) It can be seen that the surface of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 contains Ga and Fe elements, and the positions of Ga and Fe elements overlap. It can be inferred that a gallium-iron alloy is generated on the fiber surface, which also indicates the successful loading of Ga and Fe elements. The surface of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 has a gallium-iron alloy loading with obvious irregular shapes. The surface of the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 7 and 8 has a gallium-iron alloy loading with obvious irregular shapes, indicating that the gallium-iron alloy loading is successful.
[0107] The non-woven fabric testing experiment includes the following steps:
[0108] 1) In a mixed gas atmosphere of nitrogen and oxygen (the volume ratio of nitrogen to oxygen is 7:3), both sides of the non-woven fabric are plasma cleaned at 40° C. for 30 minutes (the plasma cleaning is performed under ultraviolet light in the UVC band), and a first non-woven fabric is obtained after plasma cleaning.
[0109] 2) soaking the first non-woven fabric in the gallium dispersion for 1, 2, 3, 4, and 5 times, and drying with a hair dryer at 40° C. for 40 min, to obtain gallium-containing non-woven fabrics soaked in the gallium dispersion for different times, wherein each soaking comprises: soaking in the gallium dispersion for 60 min, taking out, and drying with a hair dryer at 40° C. for 40 min.
[0110] 3) The gallium-containing non-woven fabrics soaked for different times were placed in ferrous sulfate (FeSO4) solution and soaked for 5 hours, taken out, and vacuum-dried at 80°C for 30 minutes to obtain durable gallium-iron alloy antibacterial textile fabrics soaked for different times in gallium dispersion.
[0111] Through the "non-woven fabric testing experiment", the first non-woven fabric, the gallium-containing non-woven fabric (immersed in the gallium dispersion liquid for 1 time, 2 times, 3 times, 4 times and 5 times) and the durable gallium-iron alloy antibacterial textile fabric (immersed in the gallium dispersion liquid for 1 time, 2 times, 3 times, 4 times and 5 times) can be obtained and weighed. Figure 3 (a) is a quality bar graph of the first non-woven fabric, the gallium-containing non-woven fabric, and the durable gallium-iron alloy antibacterial textile fabric; Figure 3 (b) is Figure 3 (a) The fitting curve of the Fe mass and Ga mass of the prepared gallium-iron alloy durable antibacterial textile fabric, as shown in Figure 3 (a) and (b) show that the quality of gallium-iron alloy durable antibacterial textile fabrics will increase with the increase of Ga quality and the corresponding increase of iron quality. Figure 2 It is further explained that Ga reacts with ferrous sulfate to form a mixture, and it can be inferred that the generated mixture is a gallium-iron alloy.
[0112] Through the "non-woven fabric test experiment", the first non-woven fabric, gallium-containing non-woven fabric (immersed in gallium dispersion liquid for 1 time, 2 times, 3 times, 4 times and 5 times) and durable gallium-iron alloy antibacterial textile fabric (immersed in gallium dispersion liquid for 1 time, 2 times, 3 times, 4 times and 5 times) were obtained as fabrics. The above fabrics were cut into 1*5cm strips, a 10g weight was placed on one end of the fabric, and the other end of the fabric was clamped with tweezers. It was dragged back and forth 10cm on a white paper for 20 times, 40 times and 60 times respectively, and the remaining mass after every 20 times was recorded. The original mass of the fabric ( Figure 4 The "Original mass" in the image) and the remaining mass after dragging different times ( Figure 4 "Residual mass" in Figure 4 As shown, Figure 4 (a) is the original mass of the first non-woven fabric and the gallium-containing non-woven fabric and the remaining mass after 20 draggings, Figure 4 (b) is the original mass of the first non-woven fabric and the gallium-containing non-woven fabric and the remaining mass after 40 dragging. Figure 4(c) is the original mass and the remaining mass after 60 times of dragging of the first non-woven fabric and the gallium-containing non-woven fabric, Figure 4 (d) is the original mass and the remaining mass after 20 times of dragging of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric, Figure 4 (e) is the original mass and the remaining mass after 40 times of dragging of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric, Figure 4 (f) is the original mass and the remaining mass after 60 times of dragging of the first non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric. Figure 4 From (a), (b) and (c), it can be seen that the first non-woven fabric has almost no mass loss after 20 times, 40 times and 60 times of dragging, while the gallium-containing non-woven fabric soaked with gallium dispersion solution for 1-5 times has obvious mass loss after 20 times, 40 times and 60 times of dragging, and by comparison, Figure 4 (d) and (a), Figure 4 (e) and (b), Figure 4 (f) and (c), it can be seen that the durable gallium-iron alloy antibacterial textile fabric soaked with gallium dispersion solution for 1-5 times has less mass loss after 20 times, 40 times and 60 times of dragging, which proves that soaking in ferrous sulfate solution can improve the loading stability of metal particles Ga.
[0113] Figure 5 X-ray photoelectron spectroscopy (XPS) characterization of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5, wherein (a) is the C1s spectrum, (b) is the O1s spectrum, (c) is the Ga3d spectrum, and (d) is the Fe2p spectrum. Figure 5 In (a), C1s C-O-C chemical bonds and C-C chemical bonds appear at 286eV and 285eV, respectively. Figure 5 In (b), O1s C=O chemical bonds and C-O chemical bonds appear at 532eV and 533eV, respectively, and in addition, O1s peaks overlap with sodium Auger peaks (Na KLL) at 535eV, which may be caused by O-FX bond interaction. The above analysis results characterize the C and O elements contained in the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5. Figure 5 The focus is to verify that the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 contains a variety of metal particles for antibacterial purposes, such as Ga 3+ , Ga2O3, Fe 2+ , Fe 3+ , Fe2O3, etc. Figure 5(c) shows that there are two split peaks at 18.5eV and 19eV respectively. According to the overlapping spin orbits of Ga3d, the energy difference between the two peaks is about 0.5eV, which is not much different from the standard difference Δ=0.46eV. It can be inferred that these two peaks are the split peaks of Ga element Ga3d. 3 / 2 and Ga3d 5 / 2 , and Ga appeared around 20.5eV. 3+ , Ga3d peak of Ga2O3, from which two conclusions can be drawn: after being soaked in Ga dispersion, the surface of the sample is loaded with Ga metal particles, and Ga is easily oxidized under aerobic conditions, thereby producing Ga2O3; in addition, after being soaked in FeSO4 solution, Ga and Ga2O3 undergo an electrical substitution reaction with FeSO4, thereby producing Ga 3+ , and Ga 3+ Both Ga2O3 and Mg2O3 have good antibacterial effects. Figure 5 In (d), the satellite peaks at around 735eV and 730eV belong to Fe2p 1 / 2 The satellite peaks of Fe(Ⅲ) and Fe(Ⅱ) orbitals at around 720eV and 715eV belong to Fe2p 3 / 2 The Fe(Ⅲ) and Fe(Ⅱ) orbitals appear near 709eV and 722eV respectively, which belong to Fe2p 3 / 2 and Fe2p 1 / 2 The standard energy difference between the split peaks of the high-spin compound FeO is Δ=13.1eV, which is very close to the difference between the two split peaks in the figure. 1 / 2 satellite and Fe(Ⅱ)Fe2p 3 / 2 Satellite) analysis, it can be found that there are FeO and Fe on the surface of the sample 2+ The Fe2p 3 / 2 and Fe2p 1 / 2 The orbital is always the split peak of the high spin Fe(III) compound Fe2O3, while Fe2p 3 / 2 The higher binding energy of the Fe2O3 peak (710.5eV) is not a satellite peak structure, which is due to the Fe generated by surface oxidation. 3+ The standard energy difference between the two is Δ=13.1eV. According to the Fe(Ⅲ) satellite peak (Fe(Ⅲ)Fe2p 1 / 2 Satellite and Fe(Ⅲ)Fe2p 3 / 2 The analysis of satellite showed that the sample surface contained Fe2O3 and Fe 3+ , combined with the FeO and Fe2 + There are various antibacterial particles of Fe on the surface. There is Fe2p at 706eV 3 / 2 The matal peak indicates that the sample surface contains metallic Fe. The Gibbs free energy (ΔrGm 0 )<0, due to ΔrGm 0 <0 From this, it can be inferred that Ga can spontaneously convert Fe in FeSO4 2+ Replacement to generate Ga 3+ and Fe.
[0114] Figure 6 (a) is the Fe-containing 2+ Thermogravimetric (TG) test results of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5: Figure 6 (b) is the Ga-containing antibacterial PP / PE nonwoven fabric prepared in Example 2, and the Fe-containing antibacterial PP / PE nonwoven fabric prepared in Example 4. 2+ Differential scanning calorimetry (DSC) test results of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5. The test temperature of TG is 40-800°C, the test temperature of DSC is 40-400°C, and the heating rate of both is 10°C / min. Figure 6 (a) It can be seen that the Fe 2+ The antibacterial PP / PE nonwoven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 had no significant weight loss at 100-350°C. From 350-450°C, the Fe-containing textile fabric prepared in Example 4 2+ The weight of the antibacterial PP / PE nonwoven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 both experienced a dramatic weight loss as the temperature rose. This was mainly because the organic matter in PP and PE began to oxidize and decompose at high temperatures. At 450-800°C, the weight of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 was higher than that of the Fe-containing textile fabric prepared in Example 4. 2+ Antibacterial PP / PE non-woven fabrics, proving that the thermal stability of durable gallium-iron alloy antibacterial textile fabrics (non-woven fabrics) is better than that containing Fe 2+ Antibacterial PP / PE nonwoven fabric. The Ga-containing antibacterial PP / PE nonwoven fabric prepared in Example 2 and the Fe-containing antibacterial PP / PE nonwoven fabric prepared in Example 4 2+ The melting temperature of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 is the highest, which is 168.42°C, and the corresponding melting enthalpy value is the smallest, which is 17.04 J / g. This proves that the thermal stability of the durable gallium-iron alloy antibacterial textile fabric (non-woven fabric) is better than that of the durable gallium-iron alloy antibacterial textile fabric containing Fe.2+ Antibacterial PP / PE non-woven fabric and antibacterial PP / PE non-woven fabric containing Ga.
[0115] The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE non-woven fabric containing Fe prepared in Example 3 were prepared. 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6 were placed in a fabric air permeability tester as fabrics, the pressure was set to 100 Pa, the fabric was pressed down, and the air permeability at 5 different positions was tested. The average air permeability was calculated, and the unit of the air permeability was (mm / s). Among them, the 5 different positions included the middle, the left of the middle, the right of the middle, the left and the right. Figure 7 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE non-woven fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The air permeability (average air permeability) of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6 is as follows: Figure 7 It can be seen that the antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE non-woven fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The average air permeability of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6 was not much different, and was generally maintained at 1500 mm / s.
[0116] Start the fabric moisture permeability tester and complete pre-humidification, and mix the antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE non-woven fabric containing Fe prepared in Example 3. 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 6 were fixed in a moisture permeability cup containing 25g of anhydrous calcium chloride for 1 hour, taken out and placed in a drying oven for 30 minutes, and the moisture permeability cup after drying was weighed and recorded as m1. The above-mentioned moisture permeability cup after drying was placed in a fabric moisture permeability meter for 1 hour, and the moisture permeability cup after moisture permeation was weighed and recorded as m2. The area of the moisture permeability cup is 0.00283m 2 , the moisture permeability time is 1h,
[0117] According to the formula, the moisture permeability is calculated as follows: (m2-m1) / (0.00283*h)
[0118] Figure 8 The antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial cotton fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The moisture permeability (moisture permeability) of the antibacterial PP / PE non-woven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6. Figure 8 It can be seen that the antibacterial cotton fabric containing Ga prepared in Example 1, the antibacterial PP / PE non-woven fabric containing Ga prepared in Example 2, and the antibacterial PP / PE non-woven fabric containing Fe prepared in Example 3 2+ Antibacterial pure cotton fabric, prepared in Example 4 containing Fe 2+ The moisture permeability of the antibacterial PP / PE nonwoven fabric and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6 is not much different, and is generally maintained at 4500 to 5500 g / (m 2 24h), in line with the requirements of GB 19082.
[0119] The "Non-woven Fabric Testing Experiment" yielded a first non-woven fabric and a gallium-containing non-woven fabric (immersed in a gallium dispersion solution two, three, and four times). The first non-woven fabric, the gallium-containing non-woven fabric (immersed in a gallium dispersion solution two, three, and four times), the antibacterial Ga-containing PP / PE non-woven fabric prepared in Example 2, and the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 were used to test water contact angles. The water contact angle test involved placing the fabric in a contact angle tester, adding a drop of water to the fabric surface, and measuring the water contact angle using the goniometer. The average water contact angle was then measured at different locations on the fabric. Figure 9 The water contact angle bar graphs of the first non-woven fabric, gallium-containing non-woven fabric and durable gallium-iron alloy antibacterial textile fabric are shown in FIG. Figure 9 It can be seen that after Ga loading and ferrous sulfate immersion, the water contact angle gradually decreases, but the water contact angle generally remains at around 120°, and the surface still exhibits hydrophobicity.
[0120] Antibacterial performance test method: The most important quantitative test method for antibacterial performance of textiles is the flask oscillation method. This article refers to the GB / T 20944.3 standard. Bacteria are added to the LB liquid culture medium sterilized by high temperature and high pressure to make the bacterial concentration be 10 7CFU / mL, where the bacteria are Escherichia coli (ATCC-25922) or Staphylococcus aureus (ATCC-25923). The bacteria were added to LB liquid medium and cultured at 37°C with a shaking speed of 110 rpm for 20 hours. The diluted bacterial solution was then diluted 10-fold in PBS buffer (pH = 7.4) four times.
[0121] Take 0.2g of the sample that has been disinfected by ultraviolet light and mix it with 18.6g of the diluted bacterial solution. After 20 hours of constant temperature shaking culture at 37°C, obtain the cultured bacterial solution. Take 200μl of the cultured bacterial solution, place it on a solid agar medium and spread it evenly. Place it in a constant temperature shaking incubator at 37°C and culture it for 20 hours. Take a picture to obtain the antibacterial effect diagram. Perform three parallel experiments and calculate the average value of the colony count as C1. The sample is one of the antibacterial pure cotton fabric containing Ga prepared in Example 1 and the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8.
[0122] Control group: Take 200 μl of the diluted bacterial solution and place it on solid agar medium and spread it evenly. Place it in a constant temperature shaking incubator at 37°C and incubate for 20 hours. Take a video and perform three parallel experiments. The average number of colonies is calculated as C2;
[0123] According to C1 and C2
[0124] Figure 10 The antibacterial pure cotton fabric containing Ga prepared in Example 1 and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 6 were respectively used as "samples" in the "antibacterial performance test method" to test the antibacterial effect graphs on bacteria (the bacteria are Escherichia coli or Staphylococcus aureus), wherein (a) and (b) are the antibacterial effect graphs of the control group when the bacteria are E. coli and S. aureus, (c) and (d) are the antibacterial effect graphs of the antibacterial pure cotton fabric containing Ga prepared in Example 1 on E. coli and S. aureus, (e) and (f) are the antibacterial effect graphs of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 on E. coli and S. aureus, and (g) and (h) are the antibacterial effect graphs of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 on E. coli and S. aureus. Figure 10 It can be seen that Example 1 has an antibacterial effect on E. coli and S. aureus, and the antibacterial effect of the durable gallium-iron alloy antibacterial textile fabrics prepared in Example 5 and Example 6 on E. coli and S. aureus is more obvious than the antibacterial effect of the Ga-containing antibacterial pure cotton fabric prepared in Example 1. Among them, the antibacterial effect of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 on S. aureus is the most significant.
[0125] In the above-mentioned "antibacterial performance test method", when the control group and the "sample is one of the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 6", the maximum antibacterial rate in each of the three parallel experiments is as follows: Figure 11 shown. Figure 11 (a) and (b) are the antibacterial effect diagrams of the maximum antibacterial rate of the control group against Escherichia coli and Staphylococcus aureus, (c) and (d) are the antibacterial effect diagrams of the maximum antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 against Escherichia coli and Staphylococcus aureus, (e) and (f) are the antibacterial effect diagrams of the maximum antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 against Escherichia coli and Staphylococcus aureus. Figure 11 It can be seen that the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 6 have very obvious antibacterial effects on Escherichia coli and Staphylococcus aureus, with the highest antibacterial rates reaching 99.99%.
[0126] Figure 12 The durable gallium-iron alloy antibacterial textile fabrics prepared in Example 7 and Example 8 were respectively used as the "samples" in the "antibacterial performance test method" to test the antibacterial effect of bacteria (the bacteria are Escherichia coli or Staphylococcus aureus). Among them, (a) and (b) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabrics prepared in Example 7 on E. coli and S. aureus, and (c) and (d) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabrics prepared in Example 8 on E. coli and S. aureus. Figure 12 It can be seen that compared with S. aureus, the durable gallium-iron alloy antibacterial textile fabrics prepared in Example 7 and Example 8 have a more obvious antibacterial effect on E. coli.
[0127] Figure 13 The inhibition zone effect diagram of the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 and 6 is shown. 200 μl of S. aureus bacterial solution is spread on the surface of 21-22 ml of LB solid culture medium. The S. aureus bacterial solution is prepared by pouring Staphylococcus aureus S. aureus (ATCC-25923) into LB liquid culture medium sterilized by high temperature and high pressure to make the concentration of Staphylococcus aureus S. aureus (ATCC-25923) 10 7CFU / mL, cultured at 37°C and shaking at 110 rpm for 20 hours, and diluted 10-fold twice with PBS buffer (pH 7.4). A UV-sterilized sample was placed in the LB solid medium containing the aforementioned S. aureus bacterial solution and incubated at 37°C for 20 hours to observe the formation of an inhibition zone. The sample was the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5-6. As shown in the figure, after 20 hours of incubation with the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5-6, no bacteria grew in the LB solid medium, demonstrating its excellent antibacterial effect.
[0128] Figure 14 The average antibacterial rate bar graph of the antibacterial pure cotton fabric containing Ga prepared in Example 1 and the durable gallium-iron alloy antibacterial textile fabric prepared in Examples 5 to 8 against bacteria (bacteria are Escherichia coli or Staphylococcus aureus), combined with Figures 10 to 14 The average antibacterial rate of the antibacterial pure cotton fabric containing Ga prepared in Example 1 against E. coli and S. aureus can reach 80% and 84%, the average antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 against E. coli and S. aureus can reach 88.6% and 92.5%, the average antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 against E. coli and S. aureus can reach 97.65% and 95.01%, the average antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 7 against E. coli and S. aureus can reach 95.97% and 91.92%, and the average antibacterial rate of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 8 against E. coli and S. aureus can reach 96.56% and 92.7%.
[0129] The durable gallium-iron alloy antibacterial textile fabrics prepared in Example 5 and Example 6 were washed 50 times with soapy water and steel balls (10 steel balls) (washing was performed using a water-washing color fastness tester), wherein the washing temperature was 40°C and the washing time was 45 minutes. The durable gallium-iron alloy antibacterial textile fabrics prepared in Example 5 and Example 6 after washing were respectively used as the "samples" in the aforementioned "antibacterial performance test method" for testing. The antibacterial effect is shown in the figure below. Figure 15 shown. Figure 15 (a) and (b) are the control groups of Escherichia coli and Staphylococcus aureus, respectively. (c) and (d) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 on Escherichia coli and Staphylococcus aureus after washing 50 times. (e) and (f) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 on Escherichia coli and Staphylococcus aureus after washing 50 times. Figure 15It can be seen that the durable gallium-iron alloy antibacterial textile fabrics prepared in Example 5 and Example 6 still retain a certain antibacterial effect after being washed 50 times.
[0130] The durable gallium-iron alloy antibacterial textile fabrics prepared in Example 7 and Example 8 were washed with soap water and steel balls (10 steel balls) 50 times (the washing conditions were the same as the aforementioned "washing"), wherein the washing temperature was 40°C. The durable gallium-iron alloy antibacterial textile fabrics prepared in Example 7 and Example 8 after washing were respectively used as "samples" in the aforementioned "antibacterial performance test method" for testing. The antibacterial effect diagram is shown in FIG. Figure 16 shown. Figure 16 (a) and (b) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 7 after 50 water washings on two bacteria, (c) and (d) are the antibacterial effect diagrams of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 8 after 50 water washings on two bacteria. As can be seen from the figure, Figure 12 Compared with the antibacterial effect chart, the antibacterial effect of the sample after 50 washes has decreased, but it still has obvious antibacterial effect.
[0131] Figure 17 The following is a bar graph showing the antibacterial rates of the durable gallium-iron alloy antibacterial textile fabrics prepared in Examples 5 to 8 against Escherichia coli and Staphylococcus aureus after 50 washes. The average antibacterial rates of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 after 50 washes against E. coli and S. aureus can reach 82% and 74%, respectively. The average antibacterial rates of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 after 50 washes against E. coli and S. aureus can reach 92% and 83%, respectively. The average antibacterial rates of the durable gallium-iron alloy antibacterial textile fabric (desized aramid 1414 plain weave fabric) prepared in Example 7 after 50 washes against E. coli and S. aureus can reach 84% and 82%, respectively. The average antibacterial rates of the durable gallium-iron alloy antibacterial textile fabric (desized aramid 1313 plain weave fabric) prepared in Example 8 after 50 washes against E. coli and S. aureus can reach 79% and 78%.
[0132] Use a Martindale abrasion machine to rub the sample with an original mass of m0 back and forth 10 cm 200 times with the pressure set to 200N. Weigh the sample after friction and record the mass after grinding as m.
[0133] Calculate mass loss based on m0 and m = (m0-m) / m0
[0134] Figure 18The abrasion resistance test results of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 and Example 6 are shown in Table 6. The mass loss of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 5 is 6.7% after 200 rubs, and the mass loss of the durable gallium-iron alloy antibacterial textile fabric prepared in Example 6 is only 0.8% after 200 rubs, which means that the fabric prepared in Example 6 has less abrasion and better abrasion resistance.
[0135] The above is an exemplary description of the present application. It should be noted that any simple modification, change or other equivalent replacement without creative labor of those skilled in the art without departing from the core of the present application falls within the protection scope of the present application.
Claims
1. A method for preparing a durable gallium-iron alloy antibacterial textile fabric, characterized in that: The following steps are involved: 1) plasma cleaning the textile fabric, taking it out after plasma cleaning, and soaking it in a gallium dispersion solution multiple times to obtain the gallium-containing textile fabric, wherein each soaking comprises: soaking it in the gallium dispersion solution, taking it out and drying it; 2) Soaking the gallium-containing textile fabric in a ferrous sulfate solution, taking it out, and drying it to obtain a durable antibacterial textile fabric containing a gallium-iron alloy.
2. The preparation method according to claim 1, characterized in that The textile fabric is desized pure cotton fabric, non-woven fabric or desized aramid fabric.
3. The preparation method according to claim 1, characterized in that In step 1), one or both sides of the textile fabric are plasma cleaned.
4. The preparation method according to claim 1, characterized in that In the step 1), the gallium dispersion is a mixture of metallic gallium and anhydrous ethanol, and the concentration of gallium in the gallium dispersion is 0.5-1 wt%.
5. The preparation method according to claim 1, characterized in that In the step 1), the plasma cleaning is performed in a mixed gas atmosphere of nitrogen and oxygen, and the plasma cleaning is performed under ultraviolet light irradiation in the UVC band.
6. The preparation method according to claim 1, characterized in that In the step 1), the soaking is performed 1 to 5 times.
7. The preparation method according to claim 1, characterized in that In step 2), the ferrous sulfate solution comprises: a mixture of ferrous sulfate, an antioxidant and water, the concentration of ferrous sulfate in the ferrous sulfate solution is 0.5-0.55 mol / L, and the concentration of the antioxidant in the ferrous sulfate solution is 1-2 g / L.
8. The preparation method according to claim 1, characterized in that It is characterized by: The durable gallium-iron alloy antibacterial textile fabric comprises: a textile fabric and a gallium-iron alloy loaded on the surface of the textile fabric.
9. The preparation method according to claim 8, characterized in that: Calculated by mass, the ratio of gallium to iron in the gallium-iron alloy is (1.53-2.03):
1.
10. The durable gallium-iron alloy antibacterial textile fabric obtained by the preparation method according to any one of claims 1 to 9.
11. Use of the durable gallium-iron alloy antibacterial textile fabric according to claim 10 in the preparation of antibacterial materials.
Citation Information
Patent Citations
Method for antimicrobially finishing textiles and fibers
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