CN110804868B - Mesoporous silicon composition for endowing fabric with antifouling and antibacterial properties and application thereof - Google Patents
Mesoporous silicon composition for endowing fabric with antifouling and antibacterial properties and application thereof Download PDFInfo
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- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
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Abstract
The invention relates to a mesoporous silicon composition for endowing fabric with antifouling and antibacterial properties and application thereof, which consists of antifouling mesoporous silicon spheres with antifouling functional groups on the surfaces, antibacterial mesoporous silicon spheres with antibacterial functional groups on the surfaces and polysiloxane adhesives; wherein the antifouling mesoporous silicon spheres account for 10-63% of the composition by mass, the antibacterial mesoporous silicon spheres account for 10-65% of the composition by mass, and the binder accounts for 20-45% of the composition by mass. And soaking the fabric in a tetrahydrofuran solution of the mesoporous silicon sphere composition, performing vortex oscillation for 5-20 minutes, taking out the fabric, and drying the fabric in an oven at 100-150 ℃ to obtain the super-hydrophobic antifouling antibacterial fabric. The prepared super-hydrophobic antifouling antibacterial fabric can be applied to wound application, protective masks, protective clothing and antifouling and antibacterial isolation devices. Meanwhile, the antibacterial agent has long-acting antibacterial performance; the fabric designed by the invention has wide application prospect in daily life, medical treatment and wearable equipment.
Description
Technical Field
The invention relates to a mesoporous silicon composition for endowing fabric with antifouling and antibacterial properties, which consists of antifouling mesoporous silicon spheres, antibacterial mesoporous silicon spheres and polysiloxane binder. The method is characterized in that the synergistic effect of two functionalized mesoporous silicon spheres enables the surface of the fabric to have the antifouling property of hydrophobic mesoporous silicon and the antibacterial property of quaternary ammonium salinized mesoporous silicon, and the hydrophobic mesoporous silicon can further improve the antibacterial property of quaternary ammonium mesoporous silicon on the surface of the fabric.
Background
Due to the porous structure and certain hydrophilicity of the surfaces of most fabrics, microbes such as bacteria and fungi are easy to breed, so that the negative influence is generated on the air permeability, the comfort level and the like of the fabrics, and the fabric has great danger on the health and the safety of human beings. Especially, after the skin of a human body is rubbed or scratched, microorganisms such as bacteria, fungi and the like on the fabric are easy to cause wound infection; in addition, most medical fabrics do not have good antifouling and antibacterial capabilities, and infectious diseases are easily caused after the used fabrics are not effectively sterilized. Therefore, it is very important to develop a fabric with good long-acting antifouling and antibacterial properties in medical treatment, sanitation, field operation and the like.
The preparation of the current antibacterial fabric mainly comprises two processes: the textiles are either post-treated with antimicrobial agents or some stable antimicrobial material is added to the synthetic fabric during extrusion. The antibacterial materials used in the preparation process are mainly of two types: a release-type antibacterial agent and a contact-type antibacterial agent. For the release type antibacterial material, as the antibacterial material is gradually reduced in the use process, the antibacterial performance is weakened; the contact type antibacterial material requires direct contact between microbes such as bacteria and fungi and the antibacterial material, and in the antibacterial process, live bacteria can generate metabolites and dead bacteria can remain on the surface of the fabric, which can hinder the bactericidal performance of the antibacterial material. The effective antibacterial agent mainly comprises inorganic antibacterial nanoparticles (Ag, TiO) 2ZnO, Ag @ (ZnO or SiO)2) Organic antibacterial materials (quaternary ammonium compounds (QACs), polybiguanides, N-halamines, chitosan and triclosan)) and hybrid particles (ZnO/chitosan and N-chloramine/SiO)2Etc.).
At present, a great number of researchers have conducted the design and development of antibacterial fabrics. There are two major challenges in this process: one challenge is that as part of the antibacterial fabric contains more hydroxyl functional groups and has strong water absorption, the fabric is easily polluted by sewage, and a large amount of microorganisms such as bacteria and fungi are adhered to the fabric, so that the antibacterial capability of the antibacterial fabric is reduced. Another challenge is that inorganic/organic contaminants or microorganisms such as bacteria, fungi, etc. secrete specific metabolites that are difficult to remove to form a biofilm, preventing the antimicrobial agent from coming into direct contact with the microorganisms such as bacteria, etc., resulting in a reduction in the antimicrobial ability of the fabric. In order to obtain fabrics with long-lasting antibacterial activity, many scientists have tried to design and synthesize different hydrophobic antibacterial cationic polymers, such as antibacterial materials containing quaternary ammonium salts, guanidine salts, etc., through different methods for many years. However, these fabrics finished with the antibacterial agent have only a limited antibacterial effect by reducing the adhesion of bacteria to some extent.
According to the invention, the antibacterial material is combined with the super-hydrophobic antifouling surface, so that the composition with high-efficiency antifouling and antibacterial properties is designed and used for antifouling and antibacterial modification of the fabric. The method is characterized in that polydimethylsiloxane is used as a binder, the prepared antifouling mesoporous silicon and antibacterial mesoporous silicon are combined, and the efficient antifouling and antibacterial functions of the surface of the fabric are realized through a dip-coating process.
Disclosure of Invention
The invention aims to provide a fabric treatment composition with both anti-fouling and long-acting antibacterial properties, which is mainly characterized in that two functionalized mesoporous silicon spheres are designed, and the long-acting anti-fouling and antibacterial properties are endowed to the surface of a fabric through a synergistic effect, so that the application properties of the fabric are improved.
The invention is realized by the following technical scheme:
the invention relates to a mesoporous silicon composition for endowing fabric with antifouling and antibacterial properties, which is characterized by consisting of antifouling mesoporous silicon spheres with antifouling functional groups on the surfaces, antibacterial mesoporous silicon spheres with antibacterial functional groups on the surfaces and polysiloxane binders; wherein the antifouling mesoporous silicon spheres account for 10-63% of the composition by mass, the antibacterial mesoporous silicon spheres account for 10-65% of the composition by mass, and the binder accounts for 20-45% of the composition by mass.
The composition is characterized in that the antifouling mesoporous silicon spheres are mesoporous silicon spheres containing fluorocarbon chains or mesoporous silicon spheres containing hydrophobic alkyl chains, and the average particle size of the mesoporous silicon spheres is 40-60 nm.
The composition is characterized in that the antibacterial mesoporous silicon spheres are mesoporous silicon spheres grafted with a quaternary ammonium salt antibacterial agent, the average particle size of the mesoporous silicon spheres is 30-60nm, and the Zeta potential is 20-40 mV.
The composition is characterized in that the fluorine-containing carbon chain of the mesoporous silicon sphere containing the fluorine-containing carbon chain is heptadecafluorodecyl or tridecafluorooctyl, wherein the mass content of fluorine element in the mesoporous silicon sphere is 2-20%.
The composition is characterized in that the hydrophobic alkyl chain of the mesoporous silicon sphere containing the hydrophobic alkyl chain is n-octyl or n-decyl, wherein the mass content of carbon in the mesoporous silicon sphere is 3-33%.
The composition is characterized in that the quaternary ammonium salt antibacterial agent on the antibacterial mesoporous silicon spheres is N, N-dimethyl-N- [3- (trimethicone) propyl ] octadecyl ammonium chloride, wherein the mass content of N element in the mesoporous silicon spheres is 0.08-1%.
The composition capable of endowing fabric with antifouling and antibacterial properties is characterized in that a binder in the composition is selected from Daokang medicine for curing road disease Ning-184 medicine。
The composition is formed by antifouling mesoporous silicon spheres containing heptadecafluorodecyl, N-dimethyl-N- [3- (trimethoxysilane) propyl ] octadodecyl ammonium chloride modified antibacterial mesoporous silicon spheres and Dow Corning-184.
The application method of the composition capable of endowing the fabric with the antifouling and antibacterial properties is characterized by soaking the fabric in a tetrahydrofuran solution of the mesoporous silicon sphere composition, performing vortex oscillation for 5-20 minutes, taking out the fabric, and drying the fabric in an oven at 100-150 ℃ to obtain the super-hydrophobic antifouling and antibacterial fabric.
The application of the super-hydrophobic antifouling antibacterial fabric can be applied to wound application, protective masks, protective clothing and antifouling and antibacterial isolation devices.
The antifouling mesoporous silicon spheres (FM, OM) modified by fluoridation or long alkyl chains in the antifouling and antibacterial composition are prepared by hydrolysis and alcoholysis of Tetraethoxysilane (TEOS) and trimethoxy [1H, 1H, 2H, 2H-heptadecafluorodecyl ] silane (TFDS), trimethoxy [1H, 1H, 2H, 2H-tridecafluorooctyl ] silane (TFOS), n-Octyltrimethoxysilane (OTES) or n-Decyltrimethoxysilane (DTES); the quaternary ammonium salinization antibacterial mesoporous silicon sphere (NM) is prepared by hydrolysis and alcoholysis reactions of tetraethyl orthosilicate (TEOS) and N, N-dimethyl-N- [3- (trimethoxysilane) propyl ] octadecyl ammonium chloride (TMSQ). By utilizing a dip-coating process, the Dow Corning-184 (P) is taken as a binder, the two functionalized mesoporous silicon spheres are taken as additive materials, and the roughness of the surface of the fabric (F) is combined to prepare the antifouling and antibacterial fabric with synergistic effect.
The prepared super-hydrophobic antifouling antibacterial fabric has good antifouling performance and long-acting antibacterial performance. The fabric designed by the invention has wide application prospect in daily life, medical treatment and wearable equipment.
The fabric has the super-hydrophobic antifouling antibacterial performance, is low in preparation cost, simple in preparation method and mild in reaction process, and is suitable for modification of various super-hydrophobic antifouling antibacterial functions with rough surfaces.
Drawings
FIG. 1: examples 1, 2, 7 Scanning (SEM) and Transmission (TEM) electron micrographs of unfunctionalized mesoporous silicon (a, d), quaternized mesoporous silicon (b, e), fluorinated mesoporous silicon (c, f). It can be seen from the figure that: the three nanoparticles are spherical in overall appearance, uniform in size and 30-60 nm in particle size. Compared with fluorinated mesoporous silicon, the surface of non-functionalized mesoporous silicon and quaternary ammonium salinized mesoporous silicon is smoother. The obvious radial outer pores exist in the fluorinated mesoporous silicon can be visually seen through a transmission electron microscope, and the fluorinated siloxane has microphase separation in the formation process of the mesoporous silicon, so that the pore structure exists in the silicon spheres and the surface of the silicon spheres has an obvious rough appearance.
FIG. 2: examples 1, 2, 7 infrared spectra (FTIR) of three mesoporous silicas. It can be seen from the figure that: 467cm exists in the infrared spectrogram of three mesoporous silicon -1，799cm-1，1093cm-1Three characteristic absorption peaks of Si-O-Si, wherein 3449cm-1With the vicinity of Si-OHA characteristic absorption peak; the fluorinated mesoporous silicon is 1147cm-1And 1207cm-1Presence of-CF2、-CF3The characteristic absorption peak of the quaternary ammonium salinized mesoporous silicon is 1484cm compared with the non-functionalized mesoporous silicon-1、2864cm-1And 2925cm-1The characteristic absorption peaks of-CH 2-, -CH3 exist, which are caused by more alkyl groups contained in the TMSQ molecule. And by combining Zeta potential data, the potential of non-functionalized mesoporous silicon is-9.5 mV, the potential of quaternary ammonium salinized mesoporous silicon is 24.8mV, the potential of fluorinated mesoporous silicon is-11.5 mV, the positive potential of quaternary ammonium salt enables the potential of mesoporous silicon to be converted into positive potential, and fluorine atoms can reduce the potential, so that the potential of mesoporous silicon is reduced, thereby further successfully preparing two kinds of functionalized mesoporous silicon.
FIG. 3: examples 1, 2, and 7, the energy spectrum data diagrams of fluorinated mesoporous silicon and quaternized mesoporous silicon can be qualitatively determined by mapping data diagrams of energy spectra, and both functionalized mesoporous silicon contain characteristic elements.
FIG. 4: example 25 scanning electron microscopy images and energy spectroscopy data images of the functionalized fabric surface. The untreated fabric has a smooth surface and a clear texture structure of fabric fibers; a large number of nano mesoporous silicon spheres are bonded on the surface of the fabric after the functionalization treatment, the microscopic surface of the fabric is rough, and the surface texture of the fabric fiber is covered by the silicon spheres. The surface of the fabric after the functional treatment contains the quaternary ammonium salt characteristic element (N) and the fluorosilicone characteristic element (F) is further determined by the energy spectrum data analysis of the graph (c).
FIG. 5 is a schematic view of: examples 25-31 static water contact angle plots for functionally treated fabric surfaces. As can be seen from the contact angle measurement, the surface contact angle of the fabric directly treated with polydimethylsiloxane (figure a) achieves the near-super-hydrophobic effect (133 +/-2 ℃), and the adhesion of non-functionalized mesoporous silicon to the fabric surface (figure b) also achieves the near-super-hydrophobic effect (144 +/-2 ℃), fabrics F1, F2, F3, F4, F5, F6 and F7 (figures c, d, e, F, g, h and i), and the static contact angles are 157 +/-1 DEG, 154 +/-2 DEG 152 +/-2 DEG 146 +/-3 DEG 144 +/-3 DEG 139 +/-2 DEG 136 +/-2 deg. When the proportion of the fluorinated mesoporous silicon is greater than that of the quaternary ammonium salt, the surface of the fabric has super-hydrophobic performance, the contact angle of the surface of the fabric is gradually reduced along with the increase of the proportion of the quaternary ammonium salinized mesoporous silicon, and when only the quaternary ammonium salinized mesoporous silicon exists, the contact angle of the surface of the fabric reaches 136 +/-2 degrees.
FIG. 6: the fabric treated in example 25 has excellent antifouling performance, and water, glycerin and milk can keep the droplet shape on the surface of the treated fabric and cannot infiltrate into the fabric, so that the fabric can keep good antifouling performance.
FIG. 7: example 25 scanning electron micrographs (a, b) of the stability of the functionalized fabric surface-bound nanospheres. The results in the figure illustrate that: the graph (a) is a scanning electron microscope image of the fabric which is not ultrasonically washed, and the graph (b) is a scanning electron microscope image of the fabric which is ultrasonically washed, and the graph can be obtained through the two images, the nano particles which are bonded on the surface of the functionalized fabric after being ultrasonically washed are still on the surface of the fabric, and the nano pellets are tightly bonded on the surface of the fabric through the polydimethylsiloxane.
FIG. 8: examples 25, 26, 31 air permeability of fabrics treated with different nanoparticles. A certain mass of deionized water is poured into a glass bottle, the mouth of the glass bottle is sealed by a fabric, and the glass bottle is placed at room temperature, and the mass reduction percentage of each glass bottle is measured in 10 days, 20 days and 30 days respectively. The results in the figures show that the glass bottles capped with fabric (F-P) treated with only binder dow corning-184 (P), fabric (F-P-M) bonded with non-functionalized mesoporous silicon and fabric F1, F3, F7 with different proportions of functionalized mesoporous silicon all had a mass reduction due to the evaporation of water in the bottles, and the mass reduction rates were similar, being about 4.17%, 7.67%, 14.01% in 10 days, 20 days, 30 days, respectively, compared to untreated fabric (F). This shows that the composite liquid prepared by the method has no great influence on the air permeability of the fabric.
FIG. 9: scanning electron micrographs before and after abrasion and static contact angle data plots after abrasion for the treated fabric of example 25. The graph (a) is the texture structure of the original fabric surface, the graph (b) is the texture structure of the fabric surface after 10 cycles of friction (each cycle comprises 200 times of friction), the graph (c) can observe that the contact angle of the fabric surface is gradually reduced along with the increase of the number of friction cycles, and the static water contact angle of the fabric is reduced to 131 degrees after 10 cycles of friction and still has hydrophobic property. This is probably because the fabric still has certain hydrophobic property due to the polydimethylsiloxane (P) and the functionalized mesoporous silicon which are originally adhered on the surface of the fabric after the fabric is abraded. The contact angle of the fabric is gradually reduced along with the increase of the friction cycle times, because the texture structure of the surface of the fabric is damaged every time the fabric is worn, the micro-nano structure is damaged, meanwhile, the increase of the friction cycle times also causes the non-uniform distribution of the functionalized mesoporous silicon and Dow Corning-184 (P) on the surface of the fabric, and the contact angle is gradually reduced along with the increase of the friction times.
FIG. 10: examples 25-31, anti-BSA protein adhesion experiments for fabrics were performed. The experiment shows that the adhesion amount of BSA protein on the surface of the untreated fabric is 50.842 mu gcm-2The protein adsorption amount of the fabric (F-P) treated with the polydimethylsiloxane (P) was 35.355. mu. gcm-2The BSA protein adsorption amount of the fabric adhered with the mesoporous silicon is 6.817 mu gcm-2The BSA protein adsorption amounts of fabrics F1, F2, F3, F4, F5, F6, and F7 were: 5.499 mu gcm-2，5.622μgcm-2，5.865μgcm-2，9.928 μgcm-2，9.988μgcm-2，10.861μgcm-2，11.826μgcm-2. The reduction rate of the protein adsorption amount on the surface of the fabric F3 relative to the untreated fabric reaches 88.46 percent. Through data analysis (the total added mass of the two silicon spheres is 0.6g), the protein adsorption resistance of the fabric is stronger when the ratio of the two functionalized mesoporous silicon spheres is 6:0, 5:1 and 4: 2; when the ratio is 3:3, 2:4, 1:5 and 0:6, the protein adsorption resistance of the treated fabric is gradually weakened. The reason is that when the content of FM is dominant, the FM enables the surface of the fabric to have super-hydrophobic capacity, and the surface of the fabric has stronger protein adsorption resistance; when the ratio was changed to 3:3, where NM predominated, the fabric surface did not exhibit superhydrophobic properties, and the amount of protein adhesion increased by nearly 40% over the previous. The data show that FM of the two mesoporous silicas predominates against protein adhesion, and that an increase in NM results in a decrease in the ability to resist BSA protein.
FIG. 11: example 25, fabric F1 was tested for its adhesion to e.coli as compared to a conventional antimicrobial fabric. FIG. (a) is an SEM image of untreated plain fabric adhered with E.coli, and FIG. (b) is an SEM image of fabric F1 adhered with E.coli, wherein the results show that: the untreated common fabric has a large bacterial adhesion amount, and the fabric treated by the two types of nano particles has a small bacterial adhesion amount and excellent antibacterial adhesion performance.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that various changes and modifications can be made by those skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1 preparation of non-functionalized mesoporous silicon
Preparing nanospheres: 64mL of deionized water and 9mL of absolute ethanol are mixed and dissolved in a 250mL round-bottom flask, 0.3g of Diethanolamine (DEA) is added, after stirring for 5min at 60 ℃, 10.4mL of ammonium hexadecylchloride (CTAC) with the mass fraction of 25% is added, stirring is continued for 5min, and finally 7.3g of tetraethyl orthosilicate (TEOS) is added dropwise by a constant-pressure dropping funnel, and the mixture is reacted for 3h at 60 ℃.
Centrifugal washing and drying: pouring the milky white liquid obtained by the reaction into a centrifuge tube, centrifuging for 20min at 9000rpm, taking the milky white precipitate of the lower layer, washing with water for three times, washing with alcohol for three times, and drying in a vacuum oven at 25 ℃ for 24 h.
And (3) eluting the template: grinding the dried solid into powder, pouring into prepared 500mL of methanol hydrochloric acid solution (the methanol hydrochloric acid solution is prepared according to 100mL of anhydrous methanol: 6mL of hydrochloric acid), magnetically stirring at 45 ℃ for 24h, centrifuging, washing with water and alcohol, finally placing the white precipitate in a vacuum oven at 25 ℃ and drying for 24 h.
Example 2 preparation of quaternized antibacterial mesoporous silicon
64mL of deionized water and 9mL of absolute ethanol are mixed and dissolved in a 250mL round-bottom flask, 0.2g of DEA is added, after stirring for 5min at 60 ℃, 10.4mL of 25% by mass hexadecyl ammonium chloride (CTAC) is added, stirring is continued for 5min, then 7.3g of tetraethyl orthosilicate (TEOS) and 1g of 60% by mass N, N-dimethyl-N- [3- (trimethoxysilane) propyl ] octadecyl ammonium chloride (TMSQ) isopropanol solution are added, and reaction is carried out for 5h at 30 ℃. And performing subsequent centrifugal washing, drying and template elution according to the method in the embodiment 1 to obtain the quaternary ammonium salinization antibacterial mesoporous silicon sphere NM-1. The morphology, Zeta potential, particle size, infrared spectrum, energy spectrum, etc. of NM-1 were determined as shown in Table 1 and FIGS. 1-3. The respective test methods are referred to as "measurement methods" attached later in this specification.
Examples 2 to 10
According to the method of the embodiment 2, except that the dosage of TMSQ is changed, the antibacterial mesoporous silicon spheres NM-2-5 with different quaternary ammonium salt contents (N contents) are obtained. As shown in table 1.
TABLE 1 structural Properties of antibacterial mesoporous silicon spheres prepared in examples 2-6
aContent of N element on silicon sphere in percentage by mass example 7
Preparation of mesoporous silicon ball containing fluorocarbon chain
Referring to example 1, mesoporous silicon is prepared by mixing and dissolving 64mL of deionized water and 9mL of absolute ethanol in a 250mL round-bottom flask, adding 0.2g of DEA, stirring at 60 ℃ for 5min, adding 10.4mL of 25% by mass ammonium cetylchloride (CTAC), continuing to stir for 5min, adding 7.3g of tetraethyl orthosilicate (TEOS) and 1g of trimethoxy [1H, 1H, 2H, 2H-heptadecafluorodecyl ] silane (TFDS) to mix, adding dropwise the mixture into a prepared ethanol aqueous solution, and reacting at 50 ℃ for 3H, wherein other operations in the step are kept unchanged. The subsequent drying and template elution steps are also unchanged. Obtaining the fluorinated antifouling mesoporous silicon spheres FM-1. As shown in fig. 1-3 and table 2.
Examples 7 to 15
Antifouling mesoporous silicon spheres FM-2-9 with different F element contents were obtained according to the method of example 7 and with reference to the mesoporous silicon preparation of example 1, except that the amount of TFDS was varied and trimethyloxy [1H, 1H, 2H, 2H-tridecafluorooctyl ] silane (TFOS) was used. As shown in table 2.
TABLE 2 antifouling mesoporous silica sphere structural Properties of fluorocarbon chains prepared in examples 7-15
Examples 16 to 23
The preparation method of example 7 is the same as that of example 3, except that TFDS is replaced by n-Octyltrimethoxysilane (OTES) or n-Decyltrimethoxysilane (DTES), and the amount of OTES or DTES is changed to prepare the Zeta potential and the particle size of the hydrophobic alkyl chain modified antifouling mesoporous silicon spheres OM-1-9. As shown in table 3.
TABLE 3 Properties of mesoporous silica sphere structures containing hydrophobic alkyl chains prepared in examples 7-15
Example 25
Respectively weighing 0.2g of quaternary ammonium salinization antibacterial mesoporous silicon (NM-1), 0.4g of fluorinated antifouling mesoporous silicon (FM-1) and 0.2g of A component (184-A) of adhesive Dow Corning-184 as a mesoporous silicon ball composition component I; meanwhile, 0.02g of component B (184-B) of Dow Corning-184 as a component II of the mesoporous silica sphere composition was prepared for use.
The fabric is washed with water solution of methanol and sodium hexadecyl benzene sulfonate for three times, dried and cut into 4cm × 8 cm. Adding the mesoporous silicon sphere composition component I into 20mL of tetrahydrofuran solution, carrying out ultrasonic treatment for 30min, then immersing the cut fabric into the solution, adding the mesoporous silicon sphere composition component II (0.02 g of the B component (184-B) of Dow Corning-184), carrying out vortex oscillation for 5min, taking out the fabric, placing the fabric in an oven at 130 ℃ for 6h, and drying the fabric, so that the mesoporous silicon sphere composition MC-1 endowed with the antifouling and antibacterial properties of the fabric is formed on the surface of the fabric, and the obtained fabric is numbered F3.
The Scanning Electron Microscope (SEM) image, elemental energy spectrum (Mapping), water contact angle, fabric weight gain, air permeability, adhesive strength, stain resistance, protein resistance, and antibacterial property of F3 are shown in FIGS. 4-11, and are shown in Table 4. The respective test methods are referred to as "measurement methods" attached later in this specification.
Examples 26 to 31
Mesoporous silicon sphere compositions having different compositions were prepared according to the method of example 25, except that the mass ratio of the two kinds of mesoporous silicon spheres was changed, and the compositional properties are shown in table 4 and fig. 5(b) and 9.
TABLE 4 analysis of the properties of fabrics treated with compositions prepared with different FM-1/NM-1 mass ratios
Characterize the air permeability properties of the fabric.
Examples 32 to 49
The procedure of example 25 was followed in the same manner as in example 25 except that the kind and the mass ratio of the two kinds of mesoporous silica spheres were changed to prepare mesoporous silica sphere compositions having different compositions as shown in Table 5 and properties as shown in Table 6.
TABLE 5 compositions of the compositions of examples 32-49
FM/NM/184 is the mass percentage of antifouling mesoporous silicon spheres/antibacterial mesoporous silicon spheres/Dow Corning 184 in the composition
#Characterizing the quality of the coating of the composition formed on the fabric
TABLE 6 Properties of Fabric coatings of the compositions of examples 32-49
Characterize the air permeability properties of the fabric.
The characterization method of the mesoporous silicon and the fabric performance comprises the following steps:
analyzing the mesoporous silicon appearance and the fabric surface appearance under a scanning electron microscope and analyzing an element energy spectrum:
the prepared mesoporous silicon, quaternary ammonium salinized mesoporous silicon and fluorinated mesoporous silicon are subjected to morphology characterization by using a field emission Scanning Electron Microscope (SEM) (HITACHI S-4800, Hitachi). Before SEM characterization, all samples to be tested are subjected to surface layer gold plating for 90s under the protection of argon so as to enhance the conductivity of the samples. And observing the morphology under 50-100k magnification under the conditions that the acceleration voltage is 5kV and the working distance is 10-15 mm.
When the surface appearance of the fabric is observed, the gold spraying time is prolonged to 120s, the accelerating voltage is still not 5kV, and the amplification factor is observed under the factor of 10-30 k.
And during element energy spectrum analysis, a high voltage of 15kV and a nanosphere amplification factor of 50-100k are adopted, the surface scanning is carried out for 7 times, and a final image is taken for analyzing elements and content. When the surface element of the fabric is analyzed, the voltage is 15kV, the amplification factor is 10-20k, and the damage of high voltage to the appearance of the fabric is avoided.
The mass growth rate (%) of the fabric can be calculated by equation 1:
wherein, W0For the quality of the fabric before surface treatment, W1The measurement results are taken as the mean of three parallel experiments for the mass of the treated fabric. Characterizing the amount of the mesoporous silica sphere composition on the surface modification.
Fourier infrared (FTIR) analysis:
analyzing the composition of the functional groups on the surface of the sample by using a BRUKER Vertex 70 Fourier transform infrared spectrometer, wherein the scanning range is set to 500--1. Solid samples of the nanospheres were mixed with potassium bromide, ground to a fine powder and prepared into round tablets for measurement.
Surface water contact angle test (WCA):
the surface static contact angle (WCA) before and after the treatment of the stainless steel substrate was measured using a german KRUS optical contact angle measuring instrument DSA 100. Specifically, the detection is carried out at room temperature by adopting a sitting drop method, a sample is placed on a sample table, the focal lengths of the sample and a camera are adjusted, then 5 mu L of deionized water is dropped on the surface of a base material, and the reading is carried out when the included angle between the drop and the surface of the material is constant. The test results for all samples are the mean and standard deviation of ten replicates.
Testing the antifouling performance of the fabric:
and respectively taking methyl orange dyed water, glycerol and milk as pollution solutions, dropwise adding the pollution solutions to the fabric F3 and an untreated fabric, and observing the infiltration state of liquid drops after 120 s.
And (3) testing the air permeability of the fabric:
untreated fabric, PDMS treated fabric, PDMS bonded MSNs treated fabric, fabric F1, fabric F3, fabric F7, 20mL of deionized water was added to a glass bottle having a volume of 25 mL. Cutting the fabric into a 1.5cm multiplied by 1.5cm circular shape, adhering the fabric on the glass bottle mouth by using double-sided adhesive tapes, calculating the mass reduction rate of each group of glass bottles of 10d, 20d and 30d, making five parallel samples of each fabric, and taking an average value.
Mass reduction rate calculation formula 2:
wherein M isXTotal mass of glass bottle and fabric after X days, M0The measurement results are the average of three parallel experiments for the initial mass of the glass bottles and the fabric. The greater the mass loss rate, the better the air permeability of the fabric, at the same time.
The bonding stability of the composition:
and (3) immersing the treated fabric into deionized water by using a pair of tweezers, carrying out ultrasonic treatment for 300min under the power of 180W, taking out a sample, and observing the nano particle bonding state on the surface of the fabric before and after ultrasonic treatment by using a scanning electron microscope.
Abrasion resistance test of fabric: in the practical application process, the fabric has certain abrasion, and the abrasive paper abrasion test is an effective way for evaluating the surface abrasion resistance of the material. In the experiment, silicon carbide abrasive paper and weights are used for carrying out an abrasive paper abrasion test on the fabric, and the specific method is as follows: the sample (1cm x 4cm) was placed face down over 200 mesh sandpaper, and a 200g weight was placed on the other side of the sample and moved 10cm along the scale, and then the sample was moved in reverse to the initial position, every 200 times defined as a rubbing cycle. The mechanical stability of the fabric was determined by rubbing the sample 1, 2, 3, 4, 5, 6, 7, 8, 9, 10 times to study the surface water contact angle after mechanical abrasion. The larger the water contact angle, the better the hydrophobic stability of the fabric after abrasion.
Fabric anti-protein adhesion test:
the test method adopted by the protein adsorption experiment is a BCA protein kit method. The principle is that under alkaline conditions, when BCA is combined with protein, the protein can bind Cu2+Reduction to Cu+And one Cu+It is capable of sequestering two BCA molecules, so the working reagent forms a purple complex from the original apple green and has a higher absorbance at 562nm and is proportional to the protein concentration. The protein used in this experiment was Bovine Serum Albumin (BSA) which is commonly used. According to the instruction of the BCA protein kit, a series of standard protein solutions with the concentration of 0, 2.5, 5, 10, 20, 40 and 200 mu g/mL are prepared. And (3) measuring the absorbance of the standard protein solutions at a wavelength of 562nm, and finally drawing a protein BSA standard curve by taking the absorbance as an abscissa and the protein concentration as an ordinate.
Cutting the fabric into 1cm × 4 cm; add 2mL of 2. mu.g mL into a 4mL tube-1And incubating the woven fabric in PBS (BSA) solution at 37 ℃ for 2h by a shaking table, taking out the woven fabric, quickly washing the woven fabric in 2mL of PBS, putting the woven fabric into a test tube of 2mL of PBS solution, ultrasonically washing the PBS adhered to the woven fabric for 1h, taking out the woven fabric, adding 2mL of working reagent into the test tube, incubating the test tube in an oven at 60 ℃ for 1h, cooling the test tube to room temperature, and measuring the absorbance at 562 nm. The protein adsorption amount is calculated as follows:
Wherein C is the measured protein concentration (. mu.gmL)-1) V is the volume of the phosphate buffer solution of the protein cleaning solution (2 mL is taken in the experiment), and S is the surface area (cm) of the fabric to be detected2). The greater the amount of BSA adsorbed per unit area, the weaker the anti-protein-adhesion ability of the fabric.
Testing the adhesion capability of the fabric against escherichia coli:
the invention selects escherichia coli to detect the antibacterial adhesion performance of the fabric F3. The specific experimental steps are as follows: samples (1 cm. times.1 cm) were rinsed three times with PBS, sterilized under UV light for 30 minutes, placed in 24-well plates and suspended with 1mL of bacteria (10)6CFU mL-1) And (6) covering. The cells were incubated at 37 ℃ for 4 hours. The matrix was then washed three times with PBS to remove any unattached bacteria. The bacteria were fixed with 2.5% glutaraldehyde overnight at 4 ℃, and after fixation glutaraldehyde was aspirated, rinsed gently three times with PBS, and then dehydrated continuously with 50%, 75%, 95% and 100% ethanol for 10 min. Drying the sample and observing under a scanning microscope; control-untreated fabric was not placed in bacterial suspension and the rest was performed as in experimental group. See fig. 11, three different locations on each sample were observed and the average number of adhering bacteria was counted.
Testing the antibacterial ability of the fabric:
The influence of different mass ratios of the antifouling mesoporous silicon and the antibacterial mesoporous silicon on the antibacterial performance of the fabric is explored: cutting fabric into 2cm × 2cm, and sterilizing with ultraviolet lamp for 60 min; preparing agar plates in six-well plate, and respectively configuring the concentration of Escherichia coli and Staphylococcus aureus to be 108CFU mL-1The PBS bacterial liquid of (4), and then diluting the bacterial liquid to 104CFU mL-1And putting 1mL of bacterial liquid into a six-hole plate, pressing the functional woven fabric into the six-hole plate by using a weight, taking out the fabric after 1min, putting the fabric into a new six-hole plate with the contact agar surface facing upwards, culturing in an oven at 37 ℃, and standing for 24 h. Taking out the woven fabric, carrying out vortex oscillation for 15s in 2mL PBS (phosphate buffer solution), eluting bacterial bacteria adhered to the woven fabric, taking 100 mu L of bacterial liquid for coating, culturing for 24h in a 37 ℃ incubator, and taking the average value of three parallel experiments as the counting result.
The fabric antibacterial ratio is calculated by formula 4:
the higher the antibacterial rate of the fabric is, the stronger the antibacterial performance of the fabric is.
Claims (9)
1. The application of the mesoporous silicon composition in fabric antifouling and antibacterial is characterized in that the mesoporous silicon composition consists of antifouling mesoporous silicon spheres with antifouling functional groups on the surfaces, antibacterial mesoporous silicon spheres with antibacterial functional groups on the surfaces and polysiloxane binders; wherein the antifouling mesoporous silicon spheres account for 10-63% of the composition by mass, the antibacterial mesoporous silicon spheres account for 10-65% of the composition by mass, and the binder accounts for 20-45% of the composition by mass; the antifouling mesoporous silicon spheres are mesoporous silicon spheres containing fluorocarbon chains or mesoporous silicon spheres containing hydrophobic alkyl chains, and the average particle size is 40-60 nm; the antibacterial mesoporous silicon spheres are grafted with quaternary ammonium salt antibacterial agents, and the average particle size is 30-60 nm; the fluorine-containing carbon chain of the mesoporous silicon sphere containing the fluorine-containing carbon chain is heptadecafluorodecyl or tridecafluorooctyl; the hydrophobic alkyl chain of the mesoporous silicon sphere containing the hydrophobic alkyl chain is n-octyl or n-decyl; the quaternary ammonium salt antibacterial agent on the antibacterial mesoporous silicon spheres is N, N-dimethyl-N- [3- (trimethicone) propyl ] octadecyl ammonium chloride.
2. The use of the mesoporous silicon composition of claim 1 for stain resistance and bacteria resistance of fabrics is characterized in that the Zeta potential of the antibacterial mesoporous silicon spheres is 20-40 mV.
3. The use of the mesoporous silicon composition of claim 1 for stain resistance and bacteria resistance of fabrics, wherein the fluorine content of the fluorocarbon chain-containing mesoporous silicon spheres is 2-20% by mass.
4. The use of the mesoporous silicon composition of claim 1 for stain resistance and bacteria resistance of fabrics, wherein the carbon content of the mesoporous silicon spheres containing hydrophobic alkyl chains is 3 to 33 percent by mass.
5. The application of the mesoporous silicon composition in antifouling and antibacterial fabric as claimed in claim 2, wherein the content of N element in the quaternary ammonium salt antibacterial agent on the antibacterial mesoporous silicon spheres is 0.08-1% by mass.
6. The use of a mesoporous silica composition according to claim 1 for anti-fouling and anti-bacterial applications on fabrics, characterized in that said binder is Dow Corning-184.
7. The use of the mesoporous silicon composition as recited in claim 1, wherein said mesoporous silicon composition is formed from heptadecafluorodecyl-modified antifouling mesoporous silicon spheres, N-dimethyl-N- [3- (trimethoxysilane) propyl ] octadecylammonium chloride-modified antibacterial mesoporous silicon spheres, and Dow Corning-184.
8. The use of the mesoporous silica composition of claim 1 for anti-fouling and anti-bacterial applications in protective masks, protective clothing and anti-fouling and anti-bacterial isolation devices.
9. A using method of a composition capable of endowing fabric with antifouling and antibacterial properties is characterized in that the fabric is soaked in a tetrahydrofuran solution of a mesoporous silicon composition, vortex oscillation is carried out for 5-20 minutes, then the fabric is taken out and dried in an oven at 100-150 ℃, and the super-hydrophobic antifouling antibacterial fabric is obtained; the mesoporous silicon composition consists of antifouling mesoporous silicon spheres with antifouling functional groups on the surfaces, antibacterial mesoporous silicon spheres with antibacterial functional groups on the surfaces and polysiloxane binders; wherein the antifouling mesoporous silicon spheres account for 10-63% of the composition by mass, the antibacterial mesoporous silicon spheres account for 10-65% of the composition by mass, and the binder accounts for 20-45% of the composition by mass; the antifouling mesoporous silicon spheres are mesoporous silicon spheres containing fluorocarbon chains or mesoporous silicon spheres containing hydrophobic alkyl chains, and the average particle size is 40-60 nm; the antibacterial mesoporous silicon spheres are grafted with quaternary ammonium salt antibacterial agents, and the average particle size is 30-60 nm; the fluorine-containing carbon chain of the mesoporous silicon sphere containing the fluorine-containing carbon chain is heptadecafluorodecyl or tridecafluorooctyl; the hydrophobic alkyl chain of the mesoporous silicon sphere containing the hydrophobic alkyl chain is n-octyl or n-decyl; the quaternary ammonium salt antibacterial agent on the antibacterial mesoporous silicon spheres is N, N-dimethyl-N- [3- (trimethicone) propyl ] octadecyl ammonium chloride.
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