CN112538762A - Method for preparing stable super-hydrophobic antibacterial fabric by one-pot method - Google Patents
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- D06M11/64—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with nitrogen or compounds thereof, e.g. with nitrides with nitrogen oxides; with oxyacids of nitrogen or their salts
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- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D06M13/51—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond
- D06M13/513—Compounds with at least one carbon-metal or carbon-boron, carbon-silicon, carbon-selenium, or carbon-tellurium bond with at least one carbon-silicon bond
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- D06M2200/10—Repellency against liquids
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Abstract
The invention relates to a method for preparing a stable super-hydrophobic antibacterial fabric by a one-pot method, which comprises the following steps: adding dopamine or hydrochloride thereof and a silver ion source into ethanol, carrying out ultrasonic treatment and mixing uniformly, adjusting the pH value to 8-9, adding a fluorine-free silane modifier, carrying out ultrasonic treatment and mixing uniformly to obtain a treatment solution; then soaking the cleaned and dried fabric in the treatment liquid, carrying out ultrasonic treatment, taking out the fabric treated by the treatment liquid, and drying the fabric in a heated oven; and repeating the operation for at least 3 times to obtain the stable superhydrophobic antibacterial fabric. The method is simple and time-saving, shortens the polymerization time of dopamine, simplifies the process, and ensures that the obtained fabric has higher durability and better super-hydrophobicity.
Description
Technical Field
The invention relates to the technical field of fabric surface treatment, in particular to a method for preparing a stable superhydrophobic antibacterial fabric by a one-pot method.
Background
The lotus leaf is one of the famous natural super-hydrophobic surfaces, and water drops are easy to roll on the surface of the lotus leaf and can carry away sludge along with the water drops, so that the lotus leaf has a self-cleaning effect. This is because the nano-scale hydrophobic waxy crystals are gathered on the micro-protrusions on the lotus leaf surface to form an extremely strong super-hydrophobic characteristic. The superhydrophobic property is determined by the composition of surface substances and the microstructure, and the surface with a contact angle of more than 150 ℃ and a rolling angle of less than 10 ℃ is generally defined as the superhydrophobic surface. In recent years, super-hydrophobic fabrics prepared by using soft textiles as substrates have received attention. The super-hydrophobic fabric has excellent water repellency and oil resistance and also has good self-cleaning performance.
The method for preparing the super-hydrophobic fabric is generally to construct a coarse super-nanostructure on the fabric and then modify the coarse super-nanostructure by low-surface-energy substances. The super-hydrophobic fabric has the function of inhibiting the growth and adhesion of bacteria, but has no bactericidal function. Silver ions are generally introduced for this purpose to enhance the antibacterial properties.
Zhao coats a nano silver layer on polyimide, then treats the film with potassium hydroxide and silver nitrate to perform heat treatment at 200 ℃ or higher, and finally modifies with dodecyl mercaptan (j. mater. chem, 2006, 16, 4504). Khalil Abad introduced nano silver particles composed of [ Ag (NH)3)2]+The resulting network, reduced to woven fibers, produces a superhydrophobic antimicrobial surface on cotton fabrics (j. colloid inter. sci, 2010, 351, 293). But the prepared super-hydrophobic antibacterial fabric has poor durability.
In recent years, the mussel bionic technology is widely applied to surface modification of materials, and the dopamine has extremely strong adhesion and various functional groups, so that the durability of functional fabrics can be well improved. Recently, Jianying Yang et al prepared a copper nanoparticle-coated cotton fabric by a two-step impregnation method and modified to obtain a washable super-hydrophobic antibacterial fabric (Surf Coat Technol, 2016). Jieyao Song et al soaked polydopamine fabric in modified ammonium chloride silica solution and alkyl modified to prepare washable superhydrophobic fabric (Fibers and Polymers, 2019, 7, 1380-1386). The durability of the super-hydrophobic antibacterial fabric modified by dopamine is improved, but the preparation process of the poly-dopamine is complicated, and the polymerization time of the dopamine is long.
Disclosure of Invention
In order to solve the technical problems of complex dopamine polymerization process, long polymerization time and poor fabric durability, the method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method is provided. The method can shorten the polymerization time of dopamine, simplify the process and simultaneously enable the modified fabric to have higher durability and better super-hydrophobicity.
In order to achieve the purpose, the invention is realized by the following technical scheme:
the method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method comprises the following steps:
(1) adding dopamine or hydrochloride thereof and a silver ion source into ethanol, carrying out ultrasonic treatment and mixing uniformly, adjusting the pH value to 8-9, adding a fluorine-free silane modifier, carrying out ultrasonic treatment and mixing uniformly to obtain a treatment solution;
(2) soaking the cleaned and dried fabric in the treatment solution, performing ultrasonic treatment, taking out the fabric treated by the treatment solution, and drying the fabric in a heated oven; and repeating the operation for at least 3 times to obtain the stable superhydrophobic antibacterial fabric. The super-hydrophobic effect can not be achieved after the operation is repeated for less than 3 times.
Further, the silver ion source in the step (1) is silver nitrate; the ethanol is absolute ethanol; the mass concentration of the dopamine or hydrochloride thereof in the ethanol is 6 mg/mL; the mass concentration of the silver ion source in the ethanol is 4 mg/mL-5 mg/mL.
Further, in step (1), a Tris-HCl solution with the value of 1M, pH being 8 is adopted to adjust the pH value to be 8.5.
Further, the fluorine-free silane modifier in the step (1) is hexadecyl trimethoxy silane.
Further, the amount of the fluorine-free silane modifier in the ethanol is 2 μ L/mL.
Further, the ultrasonic treatment time is 1-5 min, the ultrasonic power is 180W, and the frequency is 40 kHz.
Further, the heating temperature of the oven in the step (2) is 80-100 ℃, and preferably 100 ℃.
Further, the number of times of the repeating operation in the step (2) is 5.
The beneficial technical effects are as follows:
according to the invention, dopamine, silver ions and a fluorine-free silane modifier are directly added into ethanol, the dopamine polymerization time is shortened through Tris-HCl and high temperature, and the stable super-hydrophobic antibacterial fabric is prepared by circularly soaking and drying the fabric; compared with the method that dopamine is polymerized first and then the fluorine-free silane modifier and silver nano particle composite process is carried out, the method is simpler, more convenient and more time-saving, shortens the polymerization time of dopamine, simplifies the process, and simultaneously leads the modified fabric to have higher durability and better super-hydrophobicity.
According to the method, the super-hydrophobic surface which is self-assembled layer by layer is obtained on the surface of the fabric through cyclic soaking and drying, the nano silver and the polydopamine are compounded more firmly and are not easy to fall off, and the prepared stable super-hydrophobic antibacterial fabric has better acid resistance and washability. The modifier adopted in the method is hexadecyl trimethoxy silane, is fluorine-free, non-toxic and skin-friendly, can achieve stable super-hydrophobicity after hydrophobic modification, and has a contact angle of more than 163 degrees and a rolling angle of 5 degrees.
Drawings
Fig. 1 shows the contact angle of the stable superhydrophobic antibacterial fabric prepared in example 1 with water.
FIG. 2 is an SEM image of the surface topography of the stable superhydrophobic antibacterial fabric prepared in example 1.
Fig. 3 is a graph of Acid resistance test data of the stable superhydrophobic antibacterial fabric prepared in the example, wherein the abscissa Acid treatment time represents the Acid treatment time, the left ordinate Contact angle represents the Contact angle degree, and the right ordinate Sliding angle represents the rolling angle degree.
FIG. 4 is a graph of data of a washing resistance test of the stable superhydrophobic antibacterial fabric prepared by the example, wherein Laundering cycles represents the number of washing cycles, Contact angle on the left side represents the number of Contact angles, and Sliding angle on the right side represents the number of rolling angles.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention and the accompanying drawings, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
Example 1
The method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method comprises the following steps:
(1) adding dopamine hydrochloride and silver nitrate into 50mL of absolute ethanol to ensure that the mass concentration of the dopamine hydrochloride in the absolute ethanol is 6mg/mL and the mass concentration of the silver nitrate in the absolute ethanol is 4.8mg/mL, carrying out ultrasonic treatment for 1min, uniformly mixing, adjusting the pH value to 8.5 by using a Tris-HCl buffer solution with the concentration of 1M, pH-8, adding 100 mu L of hexadecyl trimethoxy silane, carrying out ultrasonic treatment for 5min, and uniformly mixing to obtain a treatment solution;
(2) respectively cleaning the fabric with deionized water and ethanol, and then drying in an oven at 60 ℃; soaking the cleaned and dried fabric in the treatment solution, performing ultrasonic treatment for 5min, taking out the fabric treated by the treatment solution, and drying the fabric in a drying oven at 100 ℃; and repeating the operation for 5 times to obtain the stable super-hydrophobic antibacterial fabric.
The result of the water contact angle test of the stable superhydrophobic antibacterial fabric obtained in this example is shown in fig. 1, and it can be known from fig. 1 that the contact angle of the stable superhydrophobic antibacterial fabric obtained by modifying the originally hydrophilic fabric by the method of this example with water is 163.5 ° and the roll angle is 5 °.
The surface structure of the stable superhydrophobic antibacterial fabric prepared in this example is observed by a scanning electron microscope, and an SEM image is shown in fig. 1, and it can be seen from fig. 1 that a polydopamine-nano silver complex is attached to each line on the surface of the fabric.
The fabric prepared in the embodiment is subjected to antibacterial performance detection according to GB/T20944.3-2008 (part 3: oscillation method), and the result is shown in Table 1.
TABLE 1 antimicrobial Properties of the fabrics of this example
As can be seen from Table 1, the stable superhydrophobic antibacterial fabric prepared by the present example has very good antibacterial performance.
The fabric obtained in this example was soaked in an aqueous hydrochloric acid solution having a pH of 1, taken out every 24 hours, dried, and measured for contact angle and roll angle, and the results are shown in fig. 3. As can be seen from FIG. 3, after the superhydrophobic fabric prepared by the embodiment is soaked in acid for 72 hours, the contact angle is still larger than 150 degrees, the rolling angle is smaller than 10 degrees, and the superhydrophobicity is still good, which shows that the superhydrophobic antibacterial fabric prepared by the method disclosed by the invention has good acid resistance.
The fabrics obtained in this example were subjected to a wash test according to standard procedures, AATCC test method test No. 61-20071B: 32 ℃, 10 standard stainless steel balls, 0.37 wt.% washing powder, 20 minutes as one cycle period. One cycle period is equal to five commercial or domestic washes. The results are shown in FIG. 4. As can be seen from fig. 4, after the washing test for 10 cycles, the fabric of this example still has better superhydrophobicity, which indicates that the superhydrophobic antibacterial fabric prepared by the method of the present invention has better durability.
The fabric obtained in this example was subjected to XPS elemental analysis before and after the acid soaking and washing tests. The results are shown in Table 2.
Table 2 elemental analysis comparison of fabrics before and after testing
As can be seen from the element content in Table 2, the influence of acid soaking on the antibacterial performance is small; however, the washing had a large effect on the antibacterial performance, and after washing for 10 hours (i.e., 30 cycle periods), the silver content was reduced from 1.12 wt% before the test to 0.43 wt%.
Comparative example 1
The preparation method of the super-hydrophobic antibacterial fabric of the comparative example comprises the steps of:
(1) adding dopamine hydrochloride into 50mL of deionized water to ensure that the mass concentration of the dopamine hydrochloride in the deionized water is 6mg/mL, and adjusting the pH value to 8.5 by using a Tris-HCl buffer solution with the concentration of 1M, pH-8; recording as solution A for later use;
adding silver nitrate into 50mL of deionized water to ensure that the mass concentration of the silver nitrate in the deionized water is 4.2mg/mL, and marking as a solution B for later use;
adding 100 mu L of hexadecyl trimethoxy silane into 50mL of absolute ethyl alcohol, and marking as a solution C for later use;
(2) respectively cleaning the fabric with deionized water and ethanol, then drying the fabric in a drying oven at 60 ℃, taking out the fabric, firstly soaking the cleaned and dried fabric in the solution A, placing the fabric on an HY-5A speed-regulating rotary oscillator to oscillate for 6 hours (the speed is 120rpm), carrying out self-polymerization on dopamine on the surface of the fabric in the step to obtain the fabric with polydopamine on the surface, taking out the fabric, carrying out ultrasonic treatment for 5 minutes, and drying the fabric at 60 ℃;
then immersing the fabric into the solution B for reaction for 4 hours, reducing silver ions into silver nano-ions by the polydopamine in the step to obtain the fabric with the polydopamine-silver nano-particles on the surface, taking out the fabric and drying the fabric at 60 ℃;
and finally, placing the fabric in the solution C for modification for 4 hours to obtain the super-hydrophobic antibacterial fabric prepared by the step method in the comparative example.
The fabrics obtained in the step-wise fashion of this comparative example were subjected to a wash test according to the wash test method of example 1, and AATCC test method was tested according to test No. 61-20071B: 32 ℃, 10 standard stainless steel balls, 0.37 wt.% washing powder, 20 minutes as one cycle period. One cycle period is equal to five commercial or domestic washes.
The washing test results of the superhydrophobic antibacterial fabric prepared by the one-step method of example 1 and the washing test results of the superhydrophobic antibacterial fabric prepared by the step-by-step method of this comparative example are shown in table 3.
TABLE 3 comparative data on the washability of fabrics prepared by the stepwise method and the one-pot method
As can be seen from Table 2, the contact angle of the superhydrophobic fabric prepared by the step method of comparative example 1 is smaller than that prepared by the one-pot method of the invention example 1, and the rolling angle is larger, which shows that the fabric prepared by the method of the invention has better superhydrophobicity. In addition, the fabric prepared by the step method of the comparative example 1 has a contact angle of less than 150 degrees after being washed for 2 hours, loses super-hydrophobicity, and becomes a hydrophilic surface after being washed for 4 hours; the graph in FIG. 4 shows that the contact angle of the fabric prepared by the one-pot method is reduced to less than 150 degrees after the fabric is washed for 10 hours, which shows that the washing fastness of the super-hydrophobic antibacterial fabric prepared by the method is much better than that of the fabric prepared by the step method in comparative example 1, and the super-hydrophobic antibacterial fabric has better stability.
The reasons may be: the super-hydrophobic surface prepared by the fractional step method is prepared by self-polymerizing and depositing polydopamine on the surface of the fabric, reducing silver ions into nano-silver by the weak reducibility of the polydopamine, and enabling the nano-silver to be adhered to the surface of the polydopamine due to the strong adhesiveness of the polydopamine. Then the nano silver is easy to fall off under the action of external force. The method for preparing the super-hydrophobic surface by the one-pot method is characterized in that dopamine hydrochloride is directly mixed with silver ions, so that reduced nano silver is coated by dopamine in the self-polymerization process to form a shell-core structure similar to a structure with polydopamine as a shell and silver nano particles as a core, and the coating laminated product of the polydopamine-silver nano particles is deposited on a fabric in a layer-by-layer self-assembly mode by soaking and drying in a treatment solution for multiple times. This allows a portion of the nanosilver particles to be present inside the fabric, so that a portion of the silver particles can still be present after washing. Therefore, the fabric obtained by the one-pot method of the invention has better super-hydrophobic performance, more washing resistance and better stability than the fabric obtained by the step method of the comparative example 1.
Example 2
The method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method comprises the following steps:
(1) adding dopamine hydrochloride and silver nitrate into 50mL of absolute ethanol to ensure that the mass concentration of the dopamine hydrochloride in the absolute ethanol is 6mg/mL and the mass concentration of the silver nitrate in the absolute ethanol is 4.2mg/mL, carrying out ultrasonic treatment for 1min, uniformly mixing, adjusting the pH value to 8.3 by using a Tris-HCl buffer solution with the concentration of 1M, pH-8, adding 100 mu L of hexadecyl trimethoxy silane, carrying out ultrasonic treatment for 5min, and uniformly mixing to obtain a treatment solution;
(2) respectively cleaning the fabric with deionized water and ethanol, and then drying in a 75 ℃ oven; soaking the cleaned and dried fabric in the treatment solution, performing ultrasonic treatment for 5min, taking out the fabric treated by the treatment solution, and drying the fabric in an oven at 80 ℃; and repeating the operation for 5 times to obtain the stable super-hydrophobic antibacterial fabric.
The contact angle of the stable superhydrophobic antibacterial fabric prepared in the embodiment with water is 157.1 degrees and the rolling angle is 7 degrees.
Example 3
The method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method comprises the following steps:
(1) adding dopamine hydrochloride and silver nitrate into 50mL of absolute ethanol to ensure that the mass concentration of the dopamine hydrochloride in the absolute ethanol is 6mg/mL and the mass concentration of the silver nitrate in the absolute ethanol is 4.2mg/mL, carrying out ultrasonic treatment for 1min, uniformly mixing, adjusting the pH value to 9 by using a Tris-HCl buffer solution with the concentration of 1M, pH-8, then adding 100 mu L of hexadecyl trimethoxy silane, carrying out ultrasonic treatment for 5min, and uniformly mixing to obtain a treatment solution;
(2) respectively cleaning the fabric with deionized water and ethanol, and then placing the fabric in an oven at 90 ℃ for drying; soaking the cleaned and dried fabric in the treatment solution, performing ultrasonic treatment for 5min, taking out the fabric treated by the treatment solution, and drying the fabric in a drying oven at 90 ℃; and repeating the operation for 5 times to obtain the stable super-hydrophobic antibacterial fabric.
The contact angle of the stable superhydrophobic antibacterial fabric prepared in the embodiment with water is 155.5 degrees, and the rolling angle is 8 degrees.
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Claims (8)
1. The method for preparing the stable superhydrophobic antibacterial fabric by the one-pot method is characterized by comprising the following steps of:
(1) adding dopamine or hydrochloride thereof and a silver ion source into ethanol, carrying out ultrasonic treatment and mixing uniformly, adjusting the pH value to 8-9, adding a fluorine-free silane modifier, carrying out ultrasonic treatment and mixing uniformly to obtain a treatment solution;
(2) soaking the cleaned and dried fabric in the treatment solution, performing ultrasonic treatment, taking out the fabric treated by the treatment solution, and drying the fabric in a heated oven; and repeating the operation for at least 3 times to obtain the stable superhydrophobic antibacterial fabric.
2. The one-pot method for preparing a stable superhydrophobic antibacterial fabric according to claim 1, wherein the silver ion source in step (1) is silver nitrate; the ethanol is absolute ethanol; the mass concentration of the dopamine or hydrochloride thereof in the ethanol is 6 mg/mL; the mass concentration of the silver ion source in the ethanol is 4 mg/mL-5 mg/mL.
3. The one-pot method for preparing a stable superhydrophobic antibacterial fabric according to claim 1, wherein the Tris-HCl solution with 1M, pH value of 8 is used to adjust the pH value to 8.5 in step (1).
4. The one-pot process for preparing a stable superhydrophobic and antibacterial fabric according to claim 1, wherein the fluorine-free silane modifier in step (1) is hexadecyl trimethoxysilane.
5. The one-pot method for preparing a stable superhydrophobic antibacterial fabric according to claim 1 or 4, wherein the amount of the fluorine-free silane modifier in the ethanol is 2 μ L/mL.
6. The method for preparing the stable superhydrophobic antibacterial fabric according to the one-pot method of claim 1, wherein the ultrasonic treatment time is 1-5 min, the ultrasonic power is 180W, and the frequency is 40 kHz.
7. The one-pot method for preparing the stable superhydrophobic antibacterial fabric according to claim 1, wherein the heating temperature of the oven in the step (2) is 80-100 ℃, preferably 100 ℃.
8. The one-pot method for preparing a stable superhydrophobic antibacterial fabric according to claim 1, wherein the number of times of repeating the operation in the step (2) is 5.
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Cited By (5)
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| CN112900102A (en) * | 2021-03-29 | 2021-06-04 | 安徽农业大学 | Super-hydrophobic antibacterial natural cellulose fabric and preparation method thereof |
| CN115028177A (en) * | 2022-07-08 | 2022-09-09 | 中盐淮安鸿运盐化有限公司 | Hydrophobic superfine modified anhydrous sodium sulphate and preparation method thereof |
| CN115094630A (en) * | 2021-05-21 | 2022-09-23 | 长春工业大学 | Preparation method of bio-based flame-retardant super-hydrophobic textile material |
| CN115609714A (en) * | 2022-10-21 | 2023-01-17 | 东北林业大学 | Preparation method of integral super-hydrophobic carbonized wood with environmental protection, durability, flexibility and photo-thermal functions |
| CN116751511A (en) * | 2023-05-09 | 2023-09-15 | 浙江大学 | Method for preparing super-hydrophobic coating based on polydopamine by one-pot method and obtained coating |
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