Preparation method of nano ZnO antibacterial wet tissue

Abstract

The invention discloses a preparation method of a nano ZnO antibacterial wet tissue. The method comprises the following steps: (1) performing ultraviolet soaking sterilization pretreatment on the non-woven fabric to kill various bacteria on the non-woven fabric; (2) drying the non-woven fabric treated in the step (1) to obtain a dried sterile non-woven fabric; (3) soaking the sterile non-woven fabric in the step (2) in a nano ZnO composite solution to obtain a soaked nano ZnO non-woven fabric; and (4) putting the soaked nano ZnO non-woven fabric in the step (3) into a drying oven for high-temperature fixation treatment, so that the ZnO nanoparticles are firmly attached to the non-woven fabric, and finally obtaining the nano ZnO antibacterial wet tissue. The nano ZnO antibacterial wet tissue has the advantages that the antibacterial performance of the wet tissue is improved, the wet tissue has an efficient and lasting antibacterial effect, can be in direct contact with skin, is compatible with the skin, is good in comfort level and can be used repeatedly, and the nano ZnO antibacterial wet tissue is simple in preparation process, environmentally friendly and excellent in long-acting antibacterial performance.

Description

Technical Field

[0001] The present invention relates to a preparation method of an antibacterial wet wipe, and particularly to a preparation method of a nano-ZnO antibacterial wet wipe. Background Art

[0002] Health problems such as bacterial, viral and microbial infections, as well as biological drug resistance, seriously damage human health and endanger social public safety. Pathogenic bacteria form biofilms on the surfaces of skin, glasses, mobile phones, etc. through adsorption, growth and reproduction, which not only increases the adaptability of bacteria and microorganisms to the environment, but also enhances their resistance to conventional cleaning means and disinfectants, giving rise to "super bacteria". Novel and efficient antibacterial means have become a research hotspot integrating multiple disciplines such as materials, physics, chemistry and biology.

[0003] Antibacterial wet wipes are indispensable daily necessities in modern life and play an important role in hygiene and health. Antibacterial wet wipes can help us keep our hands clean at any time when contacting public facilities, dining out or traveling, effectively kill most bacteria, and reduce the risk of pathogen transmission. In addition, antibacterial wet wipes can also be used to clean high-frequency contact items such as mobile phones and keyboards, further reducing the possibility of cross-infection.

[0004] Traditionally, conventional wet wipes are generally ethanol wet wipes. Ethanol wet wipes are popular due to the bactericidal and antibacterial properties of ethanol. However, although ethanol wet wipes have good bactericidal and antibacterial effects, due to the volatile nature of ethanol, their durability is very poor. ZnO particles have good photocatalytic activity, biocompatibility and broad-spectrum antibacterial properties, and have broad application prospects in the field of surface antibacterial. ZnO particles can generate reactive oxygen species (ROS) under light conditions, and ROS can damage the cell membranes and DNA of bacteria, thus effectively killing a variety of bacteria and microorganisms. It is precisely because ZnO particles have the above characteristics that ZnO particles are widely used in various antibacterial and bactericidal fields. However, although ZnO also has antibacterial properties and biocompatibility, since wet wipes are products that directly contact the skin, how to prepare them into antibacterial wet wipes so that they can not only maximize the antibacterial performance of the wet wipes to have efficient and long-lasting antibacterial effects, but also be able to directly contact the skin and be skin-friendly has become an urgent technical problem to be solved. Summary of the Invention

[0005] The technical problem to be solved by the invention is to provide a preparation method of a nano-ZnO antibacterial wet wipe that can not only maximize the antibacterial performance of the wet wipe to have efficient and long-lasting antibacterial effects, but also be able to directly contact the skin and be skin-friendly.

[0006] The preparation method of the nano-ZnO antibacterial wet wipe of the present invention includes the following steps:

[0007] (1) Perform ultraviolet immersion sterilization pretreatment on the non-woven fabric to kill various bacteria on the non-woven fabric;

[0008] (2) Dry the non-woven fabric processed in step (1) to obtain a dry sterile non-woven fabric;

[0009] (3) Immerse the sterile non-woven fabric in step (2) in a nano-ZnO composite solution to obtain a wet nano-ZnO non-woven fabric;

[0010] (4) Put the wet nano-ZnO non-woven fabric in step (3) into an oven for high-temperature fixation treatment to firmly attach ZnO nanoparticles to the non-woven fabric, and finally obtain a nano-ZnO antibacterial wet wipe.

[0011] Further, in step (1), the specific method of the pretreatment is: under ultraviolet light irradiation, immerse the non-woven fabric in a 75% alcohol solution for 15 - 30 min.

[0012] Still further, in step (2), the drying treatment method is: put the pretreated non-woven fabric into an oven for storage at a temperature of 60 - 80 °C.

[0013] Still further, in step (2), the drying treatment method is: put the pretreated non-woven fabric into an oven for storage with a heat preservation time of 1 - 2 h.

[0014] Still further, in step (3), the preparation method of the nano-ZnO composite solution is as follows:

[0015] Add 12.4 g of zinc acetate to 60 - 80 ml of malonic acid, and stir magnetically until clear and uniform; measure 10 - 20 mL of triethanolamine as a stabilizer, heat to 65 - 75 °C and stir; add triethanolamine to the solution in the above step and continuously stir at 65 - 75 °C for 1 - 2 h, and obtain a clear and transparent nano-ZnO composite solution after cooling.

[0016] Still further, in step (3), the immersion temperature is 30 - 40 °C, and the immersion time is 15 - 30 min.

[0017] Still further, in step (4), the temperature of the fixation treatment is 100 - 120 °C, the heat preservation time is 5 - 10 min, and after the heat preservation ends, cool to room temperature.

[0018] The non-woven fabric is a spunlace non-woven fabric.

[0019] The advantages of the present invention are:

[0020] Firstly, a nano-ZnO composite solution is prepared by chemical synthesis technology, and then a spunlace non-woven fabric is processed by soaking and fixing to obtain a nano-ZnO antibacterial wet wipe. It uses a method combining soaking and fixing to prepare the nano-ZnO antibacterial wet wipe. During the fixing process, nano-ZnO particles adhere tightly and firmly to the microstructure of the non-woven fabric, making this nano-ZnO antibacterial wet wipe not only improve the antibacterial performance of the wet wipe to the greatest extent, with high-efficiency and long-lasting antibacterial effects, but also able to be in direct contact with the skin and be skin-friendly, with good comfort, and can be reused multiple times in daily life. This nano-ZnO antibacterial wet wipe not only has a simple preparation process, is green and environmentally friendly, but also has excellent long-term antibacterial performance, and has great application prospects in public places with large traffic such as supermarkets, hospitals, and restaurants. BRIEF DESCRIPTION OF THE DRAWINGS

[0021] Figure 1 It is a schematic diagram of the preparation process for Examples 1, 2, and 3;

[0022] Figure 2 It is the microscopic structure and chemical composition of ZnO particles in Example 2; (a)-(c) are the TEM images and mapping results of nano-ZnO particles, and (d) is the energy spectrum data of nano-ZnO particles. DETAILED DESCRIPTION OF THE INVENTION

[0023] The following further elaborates in detail on the preparation method of the nano-ZnO antibacterial wet wipe of the present invention in conjunction with the drawings and specific embodiments.

[0024] The preparation method of the nano-ZnO antibacterial wet wipe of the present invention includes the following steps:

[0025] (1) Perform a pre-treatment of ultraviolet soaking and sterilization on the non-woven fabric to kill various bacteria on the spunlace non-woven fabric. Among them, the specific method of the pre-treatment is: under ultraviolet light irradiation, immerse the non-woven fabric in a 75% alcohol solution for 15 - 30 minutes. The power of the ultraviolet lamp is 15 - 40 W, the frequency is 254 nm, and the irradiance is 100 μW / cm 2 ~1000 μW / cm 2 ;

[0026] (2) Perform a drying treatment on the spunlace non-woven fabric processed in step (1) to obtain a dry sterile non-woven fabric. Among them, the drying treatment method is: put the pre-treated non-woven fabric into an oven for storage. The power of the oven is 1500 W, the temperature is 60 - 80 °C, and the heat preservation time is 1 - 2 hours;

[0027] (3) Immerse the sterile non-woven fabric in step (2) in the nano-ZnO composite solution to obtain a wet nano-ZnO non-woven fabric. Among them, the soaking temperature is 30 - 40 °C, the soaking time is 15 - 30 minutes. The preparation method of the said nano-ZnO composite solution is as follows:

[0028] Add 12.4 g of zinc acetate to 60 - 80 ml of malonic acid, and stir magnetically until clear and uniform; measure 10 - 20 mL of triethanolamine as a stabilizer, heat to 65 - 75 °C and stir; add the triethanolamine to the solution in the above step and continuously stir at 65 - 75 °C for 1 - 2 h, and obtain a clear and transparent nano - ZnO composite solution after cooling;

[0029] (4) Put the wetted nano - ZnO non - woven fabric in step (3) into an oven for high - temperature fixation treatment, so that the nano - ZnO particles are firmly attached to the non - woven fabric, and finally obtain nano - ZnO antibacterial wet wipes. Among them, the temperature of the fixation treatment is 100 - 120 °C, the heat - preservation time is 5 - 10 min, and after the heat - preservation is over, cool to room temperature.

[0030] The following combines specific examples and comparative examples to verify its effects:

[0031] Example 1

[0032] The preparation method of the nano - ZnO antibacterial wet wipes in this example includes the following steps:

[0033] (1) Carry out ultraviolet immersion sterilization pretreatment on the spunlace non - woven fabric to kill various bacteria on the non - woven fabric. The power of the ultraviolet lamp is 15 - 40 W, the frequency is 254 nm, and the irradiance is 100 μW / cm 2 ~1000 μW / cm 2 .

[0034] (2) Carry out drying treatment on the spunlace non - woven fabric treated in step (1) to obtain a dry sterile non - woven fabric. The power of the oven is 1500 W, the temperature is 60 - 80 °C, and the heat - preservation time is 1 - 2 h.

[0035] (3) Immerse the sterile non - woven fabric in step (2) in the nano - ZnO composite solution, the immersion temperature is 30 °C, and the immersion time is 15 min to obtain a wetted nano - ZnO non - woven fabric;

[0036] (4) Put the wetted nano - ZnO non - woven fabric in step (3) into an oven for high - temperature fixation treatment, the temperature of the fixation treatment is 100 °C, the heat - preservation time is 5 min, and after the heat - preservation is over, cool to room temperature to finally obtain nano - ZnO antibacterial wet wipes.

[0037] Example 2

[0038] The preparation method of the nano - ZnO antibacterial wet wipes in this example includes the following steps:

[0039] (1) Pretreat the spunlace non-woven fabric by ultraviolet immersion sterilization to kill various bacteria on the non-woven fabric. The power of the ultraviolet lamp is 15 - 40 W, the frequency is 254 nm, and the irradiance is 100 μW / cm 2 ~1000 μW / cm 2 .

[0040] (2) Dry the spunlace non-woven fabric treated in step (1) to obtain a dry sterile non-woven fabric. The power of the oven is 1500 W, the temperature is 60 - 80 °C, and the heat preservation time is 1 - 2 h.

[0041] (3) Immerse the sterile non-woven fabric in step (2) in the nano-ZnO composite solution at an immersion temperature of 40 °C for 20 min to obtain a wet nano-ZnO non-woven fabric;

[0042] (4) Put the wet nano-ZnO non-woven fabric in step (3) into the oven for high-temperature fixing treatment. The fixing temperature is 120 °C and the heat preservation time is 5 min. After the heat preservation is completed, cool it at room temperature to finally obtain the nano-ZnO antibacterial wet wipes.

[0043] Example 3

[0044] The preparation method of the nano-ZnO antibacterial wet wipes in this example includes the following steps:

[0045] (1) Pretreat the spunlace non-woven fabric by ultraviolet immersion sterilization to kill various bacteria on the non-woven fabric. The power of the ultraviolet lamp is 15 - 40 W, the frequency is 254 nm, and the irradiance is 100 μW / cm 2 ~1000 μW / cm 2 .

[0046] (2) Dry the spunlace non-woven fabric treated in step (1) to obtain a dry sterile non-woven fabric. The power of the oven is 1500 W, the temperature is 60 - 80 °C, and the heat preservation time is 1 - 2 h.

[0047] (3) Immerse the sterile non-woven fabric in step (2) in the nano-ZnO composite solution at an immersion temperature of 40 °C for 30 min to obtain a wet nano-ZnO non-woven fabric;

[0048] (4) Put the wet nano-ZnO non-woven fabric in step (3) into the oven for high-temperature fixing treatment. The fixing temperature is 120 °C and the heat preservation time is 10 min. After the heat preservation is completed, cool it at room temperature to finally obtain the nano-ZnO antibacterial wet wipes.

[0049] Comparative Example 1

[0050] The preparation method of the ethanol wet wipes includes the following steps:

[0051] (1) Pretreat the spunlace non-woven fabric by ultraviolet immersion sterilization to kill various bacteria on the non-woven fabric. The power of the ultraviolet lamp is 15 - 40 W, the frequency is 254 nm, and the irradiance is 100 μW / cm 2 ~1000 μW / cm 2 .

[0052] (2) Dry the spunlace non-woven fabric treated in step (1) to obtain a dry sterile non-woven fabric. The power of the oven is 1500 W, the temperature is 60 - 80 °C, and the heat preservation time is 1 - 2 h.

[0053] (3) Immerse the sterile non-woven fabric in step (2) in a 75% alcohol solution and stir evenly. The immersion temperature is 30 °C, the immersion time is 5 min. After the immersion, take out the wet wipes and store them sealed.

[0054] Microstructural characterization

[0055] Characterize the structure of the nano-ZnO antibacterial wet wipes in Example 2. Parameters such as the morphology and size of ZnO play an important role in the antibacterial effect. Smaller sizes enable ZnO particles to have a larger specific surface area, release more Zn 2+ ions, and generate more reactive oxygen species (ROS), thereby enhancing the antibacterial effect. As shown in Figure 2 (a)-(c), under TEM, ZnO is distributed in a granular form, and the size of a single ZnO particle is 10 1 nm level, as shown in Figure 2 (d), the Zn content in the synthesized nano-ZnO particles is 79.84%, and the O content is 20.16%.

[0056] Antibacterial performance test

[0057] According to GB 15979 - 2002 and GB / T 21510 - 2008, conduct antibacterial performance tests on the wet wipe samples prepared in Examples 1 - 3 and Comparative Example 1. Use Escherichia coli (CMCC(B)44102) and Staphylococcus aureus (CMCC(B)26003) as test strains. The concentration of the bacterial solution is 10 5 cfu / mL. Take 100 μL of the wet wipe extrusion liquid and mix it with 900 μL of the bacterial solution. After acting for a period of time, take 100 μL of the mixed solution and evenly drop it on a nutrient agar plate, and spread it evenly. At the same time, absorb 100 μL of the washing bacterial solution and perform 10 -1 times, 10 -2 times, 10 -3 times of dilution, and spread them on nutrient agar plates respectively and count. Place the plates in an incubator at 37 °C for 24 hours. Finally, calculate the sterilization rate of the samples based on the remaining colony counts in the agar plates. The test results are shown in Tables 1 and 2 below:

[0058] Table 1 Antibacterial Performance Test Results (Escherichia coli)

[0059] Bactericidal rate (%) Comparative Example 1 Example 1 Example 2 Example 3 4h 95.0 73.8 75.0 74.5 8h 93.4 85.2 87.2 86.0 12h 85.3 90.3 95.0 93.2 16h 70.5 95.4 99.9 95.5 20h 59.5 99.9 99.9 99.9 24h 35.1 100 100 100

[0060] Table 2 Antibacterial Performance Test Results (Staphylococcus aureus)

[0061] Bactericidal rate (%) Comparative Example 1 Example 1 Example 2 Example 3 4h 96.2 75.8 78.0 73.5 8h 90.4 89.3 90.2 83.4 12h 85.7 92.4 95.6 93.5 16h 73.5 99.9 99.9 99.9 20h 57.4 99.9 99.9 99.9 24h 25.1 100 100 100

[0062] From the antibacterial results in Table 1 and Table 2, it can be seen that the antibacterial rates of traditional ethanol wet wipes (Comparative Example 1) against Escherichia coli and Staphylococcus aureus within 4 hours are both greater than 95.0%, showing good antibacterial effects in a short time. When the action time exceeds 12 hours, the antibacterial effect of traditional ethanol wet wipes decreases significantly, while the antibacterial effect of nano-ZnO antibacterial wet wipes increases significantly, and the bactericidal rates against Escherichia coli and Staphylococcus aureus are both greater than 90.0%. When the action time exceeds 20 hours, the bactericidal rates of nano-ZnO antibacterial wet wipes against Escherichia coli and Staphylococcus aureus both exceed 99.9%, and the antibacterial effect is significantly better than that of traditional ethanol wet wipes, and it has excellent long-term antibacterial performance. Thus, it can be seen that by reasonably adding ZnO particles and combining with a specific preparation process, the present invention can not only improve the antibacterial performance of wet wipes, but also significantly extend their service life, which is a potential method for highly efficient and long-lasting bacteriostasis.

[0063] Of course, the above description is not a limitation of the present invention, and the present invention is not limited to the above examples. Changes, modifications, additions or substitutions made by those skilled in the art within the scope of the essence of the present invention should also fall within the protection scope of the present invention.

Claims

1. A preparation method of a nano-ZnO antibacterial wet wipe, characterized in that, It includes the following steps: (1) Pretreat the non-woven fabric by ultraviolet immersion sterilization to kill various bacteria on the non-woven fabric; (2) Dry the non-woven fabric treated in step (1) to obtain a dry sterile non-woven fabric; (3) Immerse the sterile non-woven fabric in step (2) in a nano-ZnO composite solution to obtain a wet nano-ZnO non-woven fabric; (4) Put the wet nano-ZnO non-woven fabric in step (3) into an oven for high-temperature fixing treatment to firmly attach ZnO nanoparticles to the non-woven fabric, and finally obtain a nano-ZnO antibacterial wet wipe.

2. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, wherein: In step (1), the specific method of the pretreatment is: under ultraviolet light irradiation, immerse the non-woven fabric in a 75% alcohol solution for 15 - 30 min.

3. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, wherein: In step (2), the drying treatment method is: put the pretreated non-woven fabric into an oven for storage, and the temperature is 60 - 80 °C.

4. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, characterized in that: In step (2), the drying treatment method is: put the pretreated non-woven fabric into an oven for storage, and the heat preservation time is 1 - 2 h.

5. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, wherein: In step (3), the preparation method of the nano-ZnO composite solution is as follows: Add 12.4 g of zinc acetate to 60 - 80 ml of malonic acid, and stir magnetically until clear and uniform; measure 10 - 20 mL of triethanolamine as a stabilizer, heat it to 65 - 75 °C and stir; add triethanolamine to the solution in the above step and continuously stir at 65 - 75 °C for 1 - 2 h, and obtain a clear and transparent nano-ZnO composite solution after cooling.

6. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, characterized in that: In step (3), the soaking temperature is 30 - 40 °C, and the soaking time is 15 - 30 min.

7. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, characterized in that: In step (4), the temperature of the fixing treatment is 100 - 120 °C, the heat preservation time is 5 - 10 min, and after the heat preservation ends, cool it at room temperature.

8. The preparation method of the nano-ZnO antibacterial wet wipes according to claim 1, wherein: The non-woven fabric is a spunlace non-woven fabric.

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