Preparation method of polyester fabric with antibacterial and hydrophobic properties

Through Langmuir-Blodgett technology, silane-modified silica nanoparticle film is formed on the surface of polyester fabrics. Combined with dopamine antibacterial agent, the problems of low breathable and moisture permeability and complex preparation of polyester fabrics are solved, and polyester fabrics with high efficiency antibacterial and hydrophobic properties are achieved Preparation, suitable for industrial production.

CN119308138APending Publication Date: 2025-01-14IANGSU COLLEGE OF ENG & TECH
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Patent Information

Application Number
CN202311598454.9
Authority / Receiving Office
CN · China
Patent Type
Applications(China)
Current Assignee / Owner
Filing Date
2023-11-27
Publication Date
2025-01-14

AI Technical Summary

Technical Problem

The existing polyester fabrics have low breathable and moisture permeability after functional finishing, complex preparation process and high cost, and it is difficult to balance hydrophobic and antibacterial properties in industrial production.

Method used

Langmuir-Blodgett technology is used to combine silane-modified silica nanoparticles with dopamine antibacterial agents, and a single-layer nanoparticle film is formed on the surface of the polyester fabric through low-temperature treatment, achieving efficient antibacterial and hydrophobic properties.

Benefits of technology

The preparation of polyester fabrics with efficient antibacterial and hydrophobic properties simplifies the process flow, reduces production costs, and does not require high-temperature treatment, which is suitable for industrial production.

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Abstract

The invention discloses a preparation method of a polyester fabric with antibacterial and hydrophobic properties, and belongs to the technical field of textile finishing. The method comprises the following steps: preparing silane modified silicon dioxide nanoparticles, compounding the silane modified silicon dioxide nanoparticles with a halamine antibacterial water repellent agent, preparing a monomolecular horizontal film in a steam atmosphere through Langmuir film formation, and finishing the monomolecular horizontal film on the polyester fabric through an LB method to enable the surface of the polyester fabric to have antibacterial and hydrophobic properties. The method has the advantages of simplicity in operation, high efficiency, controllable and controllable nanoparticle size and surface thickness, no need of baking treatment and the like, has small influence on the performance of the fiber, has good antibacterial and hydrophobic properties, and has wide prospects in the fields of self-cleaning, biomedicine and the like.
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Description

Technical Field

[0001] The invention belongs to the technical field of textile finishing and relates to a method for preparing polyester fabric with antibacterial and hydrophobic properties. Background Art

[0002] In recent years, inspired by the "lotus effect", the super-hydrophobic functional finishing of fabric surfaces has become a hot research field. The main feature of the super-hydrophobic phenomenon is that water drops can roll freely on the surface of super-hydrophobic textiles without wetting the surface. On the basis of hydrophobicity, textiles have multiple functions such as self-cleaning, breathability and moisture permeability. Polyester is widely used in the production of hydrophobic materials because it has a certain degree of hydrophobicity and good properties such as heat resistance and washability. The hydrophobic properties of the currently used polyester fabrics cannot meet the actual requirements, which has become a difficulty restricting the development of polyester hydrophobic fabrics. Therefore, the super-hydrophobic modification of polyester fabrics will expand the application range of polyester fabrics in the field of hydrophobic textiles.

[0003] In addition, polyester fabrics are prone to bacterial growth and reproduction during long-term use, causing mildew on the surface, which can also pose a threat to human health. Therefore, the preparation of polyester fabrics with high antibacterial and hydrophobic properties has broad application prospects. Halamine is an antibacterial material with broad-spectrum, high-efficiency, and renewable antibacterial properties, and has broad prospects in antibacterial finishing of fabrics. It is chlorinated with sodium hypochlorite, and the NH bond in the halamine group is converted into an N-Cl bond, which can inactivate bacteria in a shorter time and has excellent antibacterial properties. Dopamine has an NH structure and is a special halamine compound. In addition, it has excellent adhesion properties.

[0004] Commonly used functional finishing auxiliaries have disadvantages such as high preparation cost, high pollution and harm to human health. After hydrophobic finishing of fabrics, the fabrics often have high hydrophobic properties, but low air permeability and moisture permeability. In addition, the baking temperature during the finishing process is too high, causing damage to the fabric. It is also difficult to balance hydrophobicity and antibacterial properties, which restricts its application in industrial production. Summary of the invention

[0005] Technical issues

[0006] In view of the disadvantages of low air permeability and moisture permeability, complicated preparation process and high cost of functional finishing of current polyester fabrics, the purpose of the present invention is to provide a method for preparing polyester fabrics with antibacterial and hydrophobic properties. The method is simple and easy to implement, does not require high temperature treatment, finishes the fabric at the molecular level, and the finished polyester fabric has high efficiency antibacterial and hydrophobic properties.

[0007] Technical Solution

[0008] The present invention adopts polyester fabric (154×220 / 10cm, 400g / m2 ) is a textile material. First, a silane-modified silica nanoparticle solution is prepared, and then a certain amount of antibacterial and water-repellent agent is added to prepare a mixed solution. It is spread on the water surface of an LB (Langmuir-Blodgett) film drawing machine and placed in a certain steam atmosphere. After the solvent evaporates, a monolayer of nanoparticles is obtained. The compression area and surface pressure curve are tested by compression barrier to obtain a functional nanoparticle film. The LB technique is used to select a suitable surface pressure to transfer the polymer film to the surface of dopamine-treated polyester fabric. Dopamine plays the role of a halamine antibacterial agent and adhesion, and a polyester fabric with antibacterial and hydrophobic properties is obtained.

[0009] The present invention provides a method for preparing a polyester fabric with antibacterial and hydrophobic properties, comprising the following steps:

[0010] (1) soaking the polyester fabric in a sodium hydroxide solution, then taking it out, washing it with water, and drying it to obtain a clean polyester fabric, and then impregnating the clean polyester fabric with a dopamine solution to obtain a dopamine-treated polyester fabric;

[0011] (2) taking tetraethyl orthosilicate, silane, ammonia water, ethanol and water, mixing and reacting to prepare a silane-modified silica nanoparticle solution, and then taking an antibacterial water repellent, a silane-modified silica nanoparticle solution, a crosslinking agent and a surfactant and mixing them to prepare an antibacterial hydrophobic mixed solution;

[0012] (3) diluting the antibacterial and hydrophobic mixed solution obtained in step (2) with water to obtain a diluted solution, and then spreading the diluted solution on the water surface of an LB film drawing machine, the film surface is in a certain steam atmosphere, and sliding a barrier on the LB film drawing machine to compress at a certain speed to obtain a monolayer of nanoparticles, and then transferring the monolayer of nanoparticles to the surface of the dopamine-treated polyester fabric obtained in step (1) at a certain speed using the LB technology by a vertical pulling method or a horizontal pulling method, and then drying at a certain temperature to obtain a film-treated polyester fabric, and finally immersing the film-treated polyester fabric in a sodium hypochlorite solution for a certain period of time, and then taking it out and drying it to obtain a polyester fabric with antibacterial and hydrophobic properties.

[0013] Furthermore, the concentration of the sodium hydroxide solution in step (1) is 5-10 g / L.

[0014] Furthermore, in step (1), the polyester fabric is treated in a sodium hydroxide solution at 80-100° C. for 30-60 min.

[0015] Furthermore, the concentration of the dopamine solution in step (1) is 1 to 3 g / L.

[0016] Furthermore, in step (1), the clean polyester fabric is immersed in the dopamine solution for 5-15 minutes.

[0017] Furthermore, the silane in step (2) is one of octadecyltrimethoxysilane and hexadecyltrimethoxysilane.

[0018] Furthermore, the concentration of the ammonia water in step (2) is 25%.

[0019] Furthermore, in step (2), the volume ratio of tetraethyl orthosilicate to silane is 2:2-5.

[0020] Furthermore, in step (2), the volume ratio of tetraethyl orthosilicate to aqueous ammonia is 2:5-15.

[0021] Furthermore, in step (2), the volume ratio of tetraethyl orthosilicate to ethanol is 2:25-30.

[0022] Furthermore, in step (2), the volume ratio of tetraethyl orthosilicate to water is 2:15-25.

[0023] Furthermore, in step (2), the mixing reaction conditions of the silane-modified silica nanoparticle solution are as follows: a stirring speed of 500-2000 r / min, a reaction temperature of 50-70° C., and a reaction time of 2-5 h.

[0024] Furthermore, the antibacterial water repellent in step (2) is a polymer prepared from octavinyl POSS, hexafluorobutyl methacrylate, methacrylamide, and hydroxyethyl methacrylate.

[0025] Furthermore, the preparation method of the antibacterial water repellent described in step (2) is: octavinyl POSS (0.5-2g), hexafluorobutyl methacrylate (10-20g), methacrylamide (5-12g), hydroxyethyl methacrylate (2-5g), azobisisobutyronitrile (0.15g) and N,N-dimethylformamide (30-50mL) are mixed, and then the air is excluded, and the reaction is carried out at a temperature of 50-65°C for 9-16h, and then water is added, and then dried to obtain the antibacterial water repellent.

[0026] Furthermore, the cross-linking agent in step (2) is hexamethylene diisocyanate.

[0027] Furthermore, the surfactant in step (2) is sodium dodecylbenzene sulfonate.

[0028] Furthermore, in step (2), the mass ratio of the silane-modified silica nanoparticle solution to the antibacterial water repellent is 1:0.1-1.

[0029] Preferably, in step (2), the mass ratio of the silane-modified silica nanoparticle solution to the antibacterial water repellent is 7:3-4.

[0030] Furthermore, in step (2), the mass ratio of the silane-modified silica nanoparticle solution to the cross-linking agent is 14:0.1-1.

[0031] Furthermore, in step (2), the mass ratio of the silane-modified silica nanoparticle solution to the surfactant is 14:0.1-0.5.

[0032] Furthermore, the concentration of the diluted solution in step (3) is 1-20 mg / mL.

[0033] Furthermore, the steam atmosphere in step (3) is 80%-90%.

[0034] Furthermore, the moving speed of the sliding barrier in step (3) is 1 mm / min-10 mm / min.

[0035] Furthermore, the monomolecular film transfer speed in step (3) is 2 mm / min-10 mm / min.

[0036] Furthermore, in step (3), the number of layers of the functional nanoparticles transferred to the surface of the dopamine-treated polyester fabric is 20-40 layers.

[0037] Furthermore, the concentration of the sodium hypochlorite solution in step (3) is 10%-15%.

[0038] Furthermore, in step (3), the membrane-treated polyester fabric is treated in the sodium hypochlorite solution for 20 min to 60 min.

[0039] Furthermore, in step (3), the temperature of the two drying steps is 60-90° C., and the drying time is 10-40 min.

[0040] The invention provides a polyester fabric with antibacterial and hydrophobic properties prepared according to the method.

[0041] The invention provides an application of a polyester fabric with antibacterial and hydrophobic properties in the weaving field.

[0042] Beneficial Effects

[0043] The present invention is simple in operation and process. The method is used to prepare fluorosilane modified nanoparticles, which has the advantages of low raw material price, uniform and controllable product size and good dispersibility, and is conducive to the functional modification of silica. A molecular film with uniform and controllable surface structure is prepared by the LB method, and the modified silica and antibacterial water repellent are finished on polyester fabric. In the steam atmosphere of the polymer, water droplets can be used as a template to prepare a structure with a porous and rough morphology, which improves the hydrophobicity of the fabric surface, and the template does not need to be removed, and it can be prepared at room temperature. The selected halamine antibacterial agent has high efficiency, broad spectrum, and renewable antibacterial properties. The selected halamine antibacterial agent and dopamine have dual antibacterial effects. In actual production, the processing efficiency is high, raw materials are saved, no high temperature finishing is required, the size and surface thickness of the nanoparticles are controllable, and it has excellent hydrophobic and antibacterial properties, which can be put into industrial production. BRIEF DESCRIPTION OF THE DRAWINGS

[0044] Figure 1 Schematic diagram of LB film on polyester fabric surface.

[0045] Figure 2 This is a scanning electron micrograph of unfinished polyester fabric.

[0046] Figure 3 This is a scanning electron microscope image of the finished polyester fabric. DETAILED DESCRIPTION

[0047] The present invention will now be further described with reference to the embodiments and the accompanying drawings.

[0048] Example 1

[0049] The polyester fabric was immersed in a sodium hydroxide solution with a concentration of 10 g / L, the temperature was 90°C and the treatment time was 60 minutes, then the polyester fabric was taken out, washed with deionized water, and dried to obtain a clean polyester fabric, and then the clean polyester fabric was immersed in 2 g / L dopamine for 5 minutes to obtain a dopamine-treated polyester fabric.

[0050] Add octavinyl POSS (1g), hexafluorobutyl methacrylate (10g), methacrylamide (8g), hydroxyethyl methacrylate (3g), azobisisobutyronitrile (0.15g) and N,N-dimethylformamide (40mL) into a three-necked flask, then place the three-necked flask on an oil bath, connect a N2 tube and a condenser. First, pass N2 for 15min to evacuate the air in the device, then connect condensed water, set the oil bath temperature to 65℃, and the speed to 500rpm. When the oil bath temperature reaches 65℃, start timing, the reaction ends after 12h, the product is precipitated with deionized water, and then placed in a 50℃ vacuum oven for drying for 24h, and finally an antibacterial water repellent is obtained.

[0051] 2mL tetraethyl orthosilicate (TEOS) was used as a precursor, 4mL octadecyltrimethoxysilane was used as a modifier, 10mL 25% ammonia water, 30mL ethanol, 20mL water were added, the stirring speed was 1000r / min, the reaction temperature was 60°C, and the reaction time was 4h to obtain a silane-modified silica nanoparticle solution. 0.6g of crosslinking agent hexamethylene diisocyanate, 0.2g of surfactant sodium dodecylbenzene sulfonate, 14g of silane-modified silica nanoparticle solution and 6g of antibacterial water repellent were taken to prepare an antibacterial hydrophobic mixed solution.

[0052] The mixed solution and water were prepared into a solution with a concentration of 5 mg / mL, which was spread on the water surface of the LB (Langmuir-Blodgett) film drawing machine, in a steam atmosphere of 90%, and compressed at a speed of 3 mm / min on the LB film drawing machine to obtain a monolayer of nanoparticles. The LB technique was used to transfer it to the surface of dopamine-treated polyester fabric, and a monolayer LB film was obtained by vertical pulling at a speed of 2 mm / min. The process was repeated 20 times to obtain 20 layers of polymer monolayer-treated polyester fabric, which was dried at 80°C for 20 minutes.

[0053] Finally, the finished polyester fabric was immersed in a 10% sodium hypochlorite solution for 30 minutes and dried at 70° C. to obtain a polyester fabric with antibacterial and hydrophobic properties.

[0054] Figure 1 and Figure 2 The following are scanning electron microscope images of polyester fabric before and after finishing using the finishing method of the present invention. Figure 1 and Figure 2 It can be seen that the surface of the unfinished polyester fabric is relatively smooth and clean, without other attachments; after finishing by the finishing method of the present invention, a thin film material with a porous structure appears on the surface of the polyester fabric. The hydrophobicity of the finished polyester fabric was tested, and the contact angle was 148.6°. According to the national standard GB / T20944.3-2008, the antibacterial properties of the finished polyester fabric were measured, and the results showed that the antibacterial rate of the finished polyester fabric against Staphylococcus aureus and Escherichia coli within 5 minutes reached 100%.

[0055] Example 2

[0056] The polyester fabric with antibacterial and hydrophobic properties was prepared by referring to the method of Example 1, except that the amount of the antibacterial water repellent in Example 1 was changed to 8 g, and the other conditions or parameters were the same as those in Example 1. The contact angle of the prepared polyester fabric was 158.7°. According to the national standard GB / T20944.3-2008, the antibacterial properties of the finished polyester fabric were measured, and the results showed that the antibacterial rate of the finished polyester fabric against Staphylococcus aureus and Escherichia coli within 5 minutes reached 100%.

[0057] Example 3

[0058] The polyester fabric with antibacterial and hydrophobic properties was prepared by referring to the method of Example 1, except that the film forming times of Example 1 was changed to 40 times, and the other conditions or parameters were the same as those of Example 1. The contact angle of the prepared polyester fabric was 163.2°. According to the national standard GB / T20944.3-2008, the antibacterial properties of the finished polyester fabric were measured, and the results showed that the antibacterial rate of the finished polyester fabric against Staphylococcus aureus and Escherichia coli within 5 minutes reached 100%.

[0059] Comparative Example 1

[0060] The polyester fabric with antibacterial and hydrophobic properties was prepared by referring to the method of Example 1, except that the film forming times of Example 1 was changed to 10 times, and the other conditions or parameters were the same as those of Example 1. The contact angle of the prepared polyester fabric was 93.2°. According to the national standard GB / T20944.3-2008, the antibacterial properties of the finished polyester fabric were measured. The results showed that the antibacterial rate of the finished polyester fabric against Staphylococcus aureus within 5 minutes was 87.2%, and the antibacterial rate against Escherichia coli within 5 minutes was 85.6%. It shows that the film forming times of the LB film has an important influence on the hydrophobic and antibacterial properties of the polyester fabric.

[0061] Comparative Example 2

[0062] The polyester fabric with antibacterial and hydrophobic properties was prepared by referring to the method of Example 1, except that the concentration of the diluted solution in Example 1 was changed to 0.8 mg / mL, and the other conditions or parameters were the same as those in Example 1. The contact angle of the prepared polyester fabric was 88.9°, and it was difficult to form a porous structure on its surface. According to the national standard GB / T20944.3-2008, the antibacterial properties of the finished polyester fabric were measured, and the results showed that the antibacterial rate of the finished polyester fabric against Staphylococcus aureus within 5 minutes was 94.9%, and the antibacterial rate against Escherichia coli within 5 minutes was 96.7%. It shows that the solution concentration has an important influence on the surface morphology, hydrophobicity and antibacterial properties of the film formed on the surface of the polyester fabric.

[0063] The present invention has the following advantages:

[0064] 1. The polyester fabric prepared by the present invention has high hydrophobicity, can quickly inactivate bacteria, has high bonding strength between the finishing agent and the fiber, has simple process, high processing efficiency, low production cost, controllable nanoparticle size and surface thickness, and does not require baking treatment;

[0065] 2. The present invention optimizes the best finishing process and formula by adjusting the dosage of silane-modified silica and antibacterial and water-repellent finishing aids, controlling the finishing temperature and time. The rough porous structure prepared by the LB method and steam atmosphere can be prepared at room temperature, and the inherent properties of the polyester fabric after finishing do not change significantly. Compared with other methods, the production efficiency is improved and the added value of the product is greatly increased.

[0066] The embodiments provided above are not intended to limit the scope of the present invention, and the steps described are not intended to limit the execution order thereof. Those skilled in the art may make obvious improvements to the present invention in combination with existing common knowledge, which also fall within the scope of protection defined by the claims of the present invention.

Claims

1. A method for preparing a polyester fabric having antibacterial and hydrophobic properties, characterized in that: The following steps are involved: (1) soaking the polyester fabric in a sodium hydroxide solution, then taking it out, washing it with water, and drying it to obtain a clean polyester fabric, and then impregnating the clean polyester fabric with a dopamine solution to obtain a dopamine-treated polyester fabric; (2) taking tetraethyl orthosilicate, silane, ammonia water, ethanol and water, mixing and reacting to prepare a silane-modified silica nanoparticle solution, and then taking an antibacterial water repellent, a silane-modified silica nanoparticle solution, a crosslinking agent and a surfactant and mixing them to prepare an antibacterial hydrophobic mixed solution; (3) diluting the antibacterial and hydrophobic mixed solution obtained in step (2) with water to obtain a diluted solution, and then spreading the diluted solution on the water surface of an LB film drawing machine, the film surface is in a certain steam atmosphere, and sliding a barrier on the LB film drawing machine to compress at a certain speed to obtain a monolayer of nanoparticles, and then transferring the monolayer of nanoparticles to the surface of the dopamine-treated polyester fabric obtained in step (1) at a certain speed using the LB technology by a vertical pulling method or a horizontal pulling method, and then drying at a certain temperature to obtain a film-treated polyester fabric, and finally immersing the film-treated polyester fabric in a sodium hypochlorite solution for a certain period of time, and then taking it out and drying it to obtain a polyester fabric with antibacterial and hydrophobic properties.

2. The method according to claim 1, characterized in that In step (1), the concentration of the sodium hydroxide solution is 5-10 g / L; the parameters for treating the polyester fabric in the sodium hydroxide solution are treating at 80-100° C. for 30-60 min.

3. The method according to claim 1, characterized in that In step (1), the concentration of the dopamine solution is 1-3 g / L; the clean polyester fabric is immersed in the dopamine solution for 5-15 minutes.

4. The method according to claim 1, characterized in that In step (2), the volume ratio of tetraethyl orthosilicate to silane is 2:2-5; the volume ratio of tetraethyl orthosilicate to ammonia water is 2:5-15; the volume ratio of tetraethyl orthosilicate to ethanol is 2:25-30; and the volume ratio of tetraethyl orthosilicate to water is 2:15-25.

5. The method according to claim 1, characterized in that The antibacterial water repellent in step (2) is a polymer prepared from octavinyl POSS, hexafluorobutyl methacrylate, methacrylamide and hydroxyethyl methacrylate.

6. The method according to claim 1, characterized in that In step (2), the mass ratio of the silane-modified silica nanoparticle solution to the antibacterial water repellent is 1:0.1-1; the mass ratio of the silane-modified silica nanoparticle solution to the crosslinking agent is 14:0.1-1; and the mass ratio of the silane-modified silica nanoparticle solution to the surfactant is 14:0.1-0.

5.

7. The method according to claim 1, characterized in that In step (3), the concentration of the diluted solution is 1-20 mg / mL; and the steam atmosphere is 80%-90%.

8. The method according to claim 1, characterized in that In step (3), the sliding barrier moving speed is 1mm / min-10mm / min; the monomolecular film transfer speed is 2mm / min-10mm / min; and the number of layers of functional nanoparticles transferred to the dopamine-treated polyester fabric surface is 20-40 layers.

9. A polyester fabric with antibacterial and hydrophobic properties obtained by the method according to any one of claims 1 to 8.

10. Use of the polyester fabric with antibacterial and hydrophobic properties as claimed in claim 9 in the weaving field.

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