CN113875775A - Preparation method of all-silicon molecular sieve packaged nano-silver bactericide - Google Patents
Preparation method of all-silicon molecular sieve packaged nano-silver bactericide Download PDFInfo
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N59/00—Biocides, pest repellants or attractants, or plant growth regulators containing elements or inorganic compounds
- A01N59/16—Heavy metals; Compounds thereof
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
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- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Abstract
The invention belongs to the technical field of bactericide preparation, and particularly relates to a preparation method of a nano-silver bactericide packaged by a full-silicon molecular sieve. On one hand, the coordination of (3-mercaptopropyl) trimethoxysilane and silver ions is utilized to prevent the silver ions from precipitating, and the interaction between the trimethoxysilane and a molecular sieve precursor is utilized to uniformly disperse the silver ions in the pore channels of the molecular sieve. On the other hand, the limited aperture of the molecular sieve can also effectively limit the release rate of silver ions, avoid the occurrence of the burst release phenomenon, achieve the purpose of slow release, and enable the silver ion to have wide application prospect as a broad-spectrum bactericide.
Description
Technical Field
The invention belongs to the technical field of preparation of nano-silver bactericides, and particularly relates to a preparation method of a nano-silver bactericide packaged by an all-silicon molecular sieve.
Background
The research shows that the surface of nano silver in water or water-containing air can be oxidized to free micro silver ions, and when the concentration of the silver ions reaches 0.01ppm, the nano silver has a good sterilization effect, and after bacteria die, the silver ions can be released to continuously play a sterilization function, so that the nano silver is a high-quality and long-acting bactericide. However, if nano silver is directly used for sterilization, the problems of high price, easy aggregation, unstable release and the like exist, and for many years, scientists have tried to uniformly load nano silver into various carriers to obtain better sterilization effect.
The molecular sieve is a crystalline silicate or aluminosilicate, has a regular structure and good thermal and hydrothermal stability, and meanwhile, narrow pore channels of the molecular sieve can effectively prevent silver nanoparticles from aggregating and control the release rate of the silver nanoparticles, so that the molecular sieve is an ideal carrier for the sustained and controlled release of the Ag bactericide.
Currently, some research progress has been made in the encapsulation of nano silver by molecular sieves. For example, there are studies on the successful synthesis of Ag-TiO by a novel two-step hydrothermal method2Nanotube composite material made of nanotube TiO2The structural composition is that Ag nano particles are uniformly dispersed in the whole material, the particle size is about 3nm, but the scanning electron microscope result shows that 32 to 103nm of silver nano particles are dissociated on the outer side of the material. It has also been studied to pack Ag nanoparticles into hollow ZSM-5 molecular sieve crystals by conventional impregnation or to locate Ag clusters in the channels of the molecular sieve by ion exchange. Although the molecular sieve encapsulated nano-silver bactericide can be synthesized by the method, a part of metal precursors is inevitable in the loading processThe Ag is adsorbed on the outer surface of the carrier or the framework, so that the distribution of Ag is uneven, the release rate of the Ag bactericide is too high, and the bactericidal performance is finally influenced.
Therefore, a new preparation method of the molecular sieve encapsulated nano-silver bactericide with strong universality needs to be developed so as to improve the bactericidal activity and controllable release rate of the nano-silver bactericide.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention provides a preparation method of an all-silicon molecular sieve encapsulated nano-silver bactericide, the prepared bactericide consists of an all-silicon molecular sieve carrier and an active component loaded on the carrier, the active component is silver nanoparticles, and nano-silver metal is uniformly dispersed in the carrier. The reaction system related to the preparation method is simple, the reaction condition is mild, and the obtained all-silicon molecular sieve encapsulated nano-silver bactericide has a novel structure, higher bactericidal activity and controllable release rate, and has wide application prospect as a broad-spectrum bactericide.
In order to achieve the purpose, the invention adopts the technical scheme that:
the invention provides a preparation method of an all-silicon molecular sieve encapsulated nano-silver bactericide, which comprises the following steps:
s1, adding water into the tetrapropyl ammonium hydroxide solution for dilution, adding (3-mercaptopropyl) trimethoxysilane into the solution to prepare a mixed solution, adding a silver nitrate water solution into the mixed solution, and continuously stirring for more than 30 minutes;
s2, adding tetraethyl silicate into the mixed system obtained in the step S1 to obtain silver-silica sol, and aging the silver-silica sol to obtain silver-silica gel;
s3, statically crystallizing the silver-silicon gel obtained in the step S2, roasting at high temperature in the air atmosphere, and reducing at high temperature in the hydrogen atmosphere to finally obtain the all-silicon molecular sieve packaged nano silver bactericide.
Preferably, the temperature of the static crystallization is 90-125 ℃, and the time is 48-144 hours. Specifically, the static crystallization was static crystallization at 95 ℃ for 4 days.
Preferably, the high-temperature roasting temperature is 300-550 ℃, the time is 1-8 hours, and the heating rate is 0.5-5 ℃/min. Specifically, the high-temperature roasting temperature is 500 ℃, the time is 2 hours, and the heating rate is 0.5 ℃/min.
Preferably, the high-temperature reduction is carried out at the temperature of 250-500 ℃ for 2-4 hours at the temperature rise rate of 0.5-5 ℃/min. Specifically, the temperature of the high-temperature reduction is 300 ℃, the time is 2 hours, and the heating rate is 0.5 ℃/min.
Preferably, the aging temperature is 40-90 ℃ and the aging time is 1-2 hours. Specifically, the temperature of the aging is 80 ℃ and the time is 1 hour.
Preferably, in step S1, the tetrapropylammonium hydroxide solution has a concentration of 25 wt% to 40 wt%, and the silver nitrate aqueous solution has a concentration of 0.2 wt% to 0.3 wt%, and is diluted with water so that the silver-silica sol obtained in step S2 has a tetrapropylammonium hydroxide concentration of 9.0 wt% to 10.0 wt%, and a silver nitrate concentration of 0.06 wt% to 0.08 wt%.
Preferably, the molar ratio of the tetrapropylammonium hydroxide to the tetraethyl silicate is 1: 2-5.
Preferably, the molar ratio of silver nitrate to (3-mercaptopropyl) trimethoxysilane is 1:10 to 40.
Preferably, the molar ratio of the tetrapropylammonium hydroxide to the (3-mercaptopropyl) trimethoxysilane is 1: 0.15-0.25.
The invention also provides the all-silicon molecular sieve encapsulated nano-silver bactericide prepared by the preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide.
Compared with the prior art, the invention has the beneficial effects that:
the invention provides a preparation method of a nano-silver bactericide packaged by a full-silicon molecular sieve, which comprises the steps of introducing a nano-silver precursor complex formed by (3-mercaptopropyl) trimethoxysilane and silver nitrate into a synthesis system of the full-silicon molecular sieve, packaging a nano-silver precursor into the full-silicon molecular sieve through in-situ static crystallization, and finally preparing the nano-silver bactericide packaged by the full-silicon molecular sieve through high-temperature roasting and hydrogen reduction. On one hand, the coordination effect of (3-mercaptopropyl) trimethoxysilane and silver ions is utilized to protect the silver ions and prevent the silver ions from precipitating in alkaline sol for synthesizing the molecular sieve, and the interaction between the (3-mercaptopropyl) trimethoxysilane and a molecular sieve precursor is utilized to lead the silver ions to be encapsulated into the pore canal of the molecular sieve in the synthesis process, thereby avoiding the aggregation of the silver ions on the outer surface of the molecular sieve to the maximum extent and being beneficial to the uniform dispersion of the silver ions in the pore canal of the molecular sieve. On the other hand, the limited aperture of the molecular sieve can also effectively limit the release rate of silver ions, avoid the occurrence of the burst release phenomenon, achieve the purpose of slow release, can be used as a broad-spectrum bactericide, and has wide application prospect.
Drawings
FIG. 1 is an XRD diagram of an all-silicon molecular sieve encapsulated nano-silver bactericide;
FIG. 2 is a TEM image of the all-silicon molecular sieve encapsulated nano-silver bactericide.
Detailed Description
The following further describes the embodiments of the present invention. It should be noted that the description of the embodiments is provided to help understanding of the present invention, but the present invention is not limited thereto. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The experimental procedures in the following examples were carried out by conventional methods unless otherwise specified, and the test materials used in the following examples were commercially available by conventional methods unless otherwise specified.
Example 1 preparation of all-silica molecular sieve encapsulated nano-silver bactericide (Silicalite-1 molecular sieve as molecular sieve carrier)
(1) 7.32g of aqueous tetrapropylammonium hydroxide solution (TPAOH, 40 wt%) were added 5g H2Diluting O, adding 0.507mL (3-mercaptopropyl) trimethoxysilane, and uniformly mixing to prepare a mixed solution; 0.022g of silver nitrate (AgNO) is taken3) Adding 7.887gH2Dissolving the O into silver nitrate aqueous solution, dripping the obtained silver nitrate aqueous solution into the mixed solution, and continuously stirring for 30 minutes.
(2) And dropwise adding 10g of tetraethyl silicate (TEOS) into the mixed system, uniformly mixing to obtain colorless and transparent silver-silica sol, heating the obtained silver-silica sol to 80 ℃, stirring and aging for 1h to obtain the silver-silica gel.
(3) And (2) placing the silver-silicon gel into a crystallization kettle with a polytetrafluoroethylene lining, performing static crystallization for 4 days at 95 ℃, centrifuging, washing and drying after crystallization is finished, transferring the obtained sample into a tubular furnace, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (the heating rate is 0.5 ℃/min), cooling to room temperature after roasting, then heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (the heating rate is 0.5 ℃/min), thus obtaining the all-silicon molecular sieve packaged nano silver bactericide (Ag @ Silicalite-1).
The prepared all-silicon molecular sieve encapsulated nano-silver bactericide is subjected to X-ray diffraction (XRD) and Transmission Electron Microscope (TEM) analysis, and the XRD data in figure 1 show that the self structure of the encapsulated Silicalite-1 molecular sieve is not obviously influenced. As can be seen from the data of the transmission electron microscope in FIG. 2, the Ag nanoparticles are uniformly dispersed in the Silicalite-1 molecular sieve crystals, and the particle size is about 1-2 nm.
Embodiment 2 preparation method of all-silicon molecular sieve encapsulated nano-silver bactericide
(1) 7.32g of aqueous tetrapropylammonium hydroxide solution (TPAOH, 40 wt%) were added 5g H2Diluting O, adding 0.622mL (3-mercaptopropyl) trimethoxysilane, and uniformly mixing to prepare a mixed solution; taking 0.027g of silver nitrate (AgNO)3) Adding 7.887g H2Dissolving the O into silver nitrate aqueous solution, dripping the obtained silver nitrate aqueous solution into the mixed solution, and continuously stirring for 30 minutes.
(2) And dropwise adding 10g of tetraethyl silicate (TEOS) into the mixed system, uniformly mixing to obtain colorless and transparent silver-silica sol, heating the obtained silver-silica sol to 80 ℃, stirring and aging for 1h to obtain the silver-silica gel.
(3) And (2) placing the silver-silicon gel into a crystallization kettle with a polytetrafluoroethylene lining, performing static crystallization for 4 days at 95 ℃, centrifuging, washing and drying after crystallization is finished, transferring the obtained sample into a tubular furnace, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (the heating rate is 0.5 ℃/min), cooling to room temperature after roasting, then heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (the heating rate is 0.5 ℃/min), thus obtaining the all-silicon molecular sieve packaged nano silver bactericide.
The XRD and TEM analysis results are consistent with example 1.
Example 3 preparation method of all-silicon molecular sieve encapsulated nano-silver bactericide
(1) 7.32g of aqueous tetrapropylammonium hydroxide solution (TPAOH, 40 wt%) were added 5g H2Diluting O, adding 0.761mL (3-mercaptopropyl) trimethoxysilane, and uniformly mixing to prepare a mixed solution; 0.033g of silver nitrate (AgNO) is taken3) Adding 7.887g H2Dissolving the O into silver nitrate aqueous solution, dripping the obtained silver nitrate aqueous solution into the mixed solution, and continuously stirring for 30 minutes.
(2) And dropwise adding 10g of tetraethyl silicate (TEOS) into the mixed system, uniformly mixing to obtain colorless and transparent silver-silica sol, heating the obtained silver-silica sol to 80 ℃, stirring and aging for 1h to obtain the silver-silica gel.
(3) And (2) placing the silver-silicon gel into a crystallization kettle with a polytetrafluoroethylene lining, performing static crystallization for 4 days at 95 ℃, centrifuging, washing and drying after crystallization is finished, transferring the obtained sample into a tubular furnace, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (the heating rate is 0.5 ℃/min), cooling to room temperature after roasting, then heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (the heating rate is 0.5 ℃/min), thus obtaining the all-silicon molecular sieve packaged nano silver bactericide.
The XRD and TEM analysis results are consistent with example 1.
Example 4 preparation method of all-silicon molecular sieve encapsulated nano-silver bactericide
(1) 7.32g of aqueous tetrapropylammonium hydroxide solution (TPAOH, 40 wt%) were added 5g H2Diluting O, adding 1.153mL (3-mercaptopropyl) trimethoxysilane, and uniformly mixing to prepare a mixed solution; 0.05g of silver nitrate (AgNO) is taken3) Adding 7.887gH2Dissolving the O into silver nitrate aqueous solution, dripping the obtained silver nitrate aqueous solution into the mixed solution, and continuously stirring for 30 minutes.
(2) And dropwise adding 10g of tetraethyl silicate (TEOS) into the mixed system, uniformly mixing to obtain colorless and transparent silver-silica sol, heating the obtained silver-silica sol to 80 ℃, stirring and aging for 1h to obtain the silver-silica gel.
(3) And (2) placing the silver-silicon gel into a crystallization kettle with a polytetrafluoroethylene lining, performing static crystallization for 4 days at 95 ℃, centrifuging, washing and drying after crystallization is finished, transferring the obtained sample into a tubular furnace, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (the heating rate is 0.5 ℃/min), cooling to room temperature after roasting, then heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (the heating rate is 0.5 ℃/min), thus obtaining the all-silicon molecular sieve packaged nano silver bactericide.
The XRD and TEM analysis results are consistent with example 1.
Example 5 preparation method of all-silicon molecular sieve encapsulated nano-silver bactericide
(1) 7.32g of aqueous tetrapropylammonium hydroxide solution (TPAOH, 40 wt%) were added 5g H2Diluting O, adding 0.577mL (3-mercaptopropyl) trimethoxysilane, and uniformly mixing to prepare a mixed solution; 0.25g of silver nitrate (AgNO) is taken3) Adding 7.887gH2Dissolving the O into silver nitrate aqueous solution, dripping the obtained silver nitrate aqueous solution into the mixed solution, and continuously stirring for 30 minutes.
(2) And dropwise adding 10g of tetraethyl silicate (TEOS) into the mixed system, uniformly mixing to obtain colorless and transparent silver-silica sol, heating the obtained silver-silica sol to 80 ℃, stirring and aging for 1h to obtain the silver-silica gel.
(3) And (2) placing the silver-silicon gel into a crystallization kettle with a polytetrafluoroethylene lining for static crystallization at 95 ℃ for 4 days, centrifuging, washing and drying after crystallization is finished, transferring the obtained sample into a tubular furnace, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (the heating rate is 0.5 ℃/min), cooling to room temperature after roasting, then heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (the heating rate is 0.5 ℃/min), thus obtaining the all-silicon molecular sieve packaged nano silver bactericide.
The XRD and TEM analysis results are consistent with example 1.
Comparative example 1 all-silica molecular sieve loaded with nano-silver by impregnation
Soaking 5g of all-silicon molecular sieve (Silicalite-1 molecular sieve) in 10mL of silver nitrate aqueous solution (0.16 wt%), evaporating to remove water, heating to 500 ℃ in the air atmosphere, roasting for 2 hours (heating rate of 0.5 ℃/min), cooling to room temperature, heating to 300 ℃ in the hydrogen atmosphere, and reducing for 2 hours (heating rate of 0.5 ℃/min) to obtain the all-silicon molecular sieve loaded with nano silver by adopting an impregnation method.
Experimental example 1 silver ion Release Rate test
The silver ion release rates of the all-silicon molecular sieves of examples 1 and 2 were tested by taking the all-silicon molecular sieves encapsulating the nano-silver bactericide as an example and taking a sample of the all-silicon molecular sieve loading the nano-silver by an immersion method as a control.
The all-silica molecular sieve encapsulated nano-silver samples of examples 1 and 2 and the all-silica molecular sieve sample loaded with nano-silver by an immersion method (each sample contains about 0.4mg of nano-silver calculated by silver content) were weighed into a 50mL centrifuge tube, 20mL of absolute ethanol was added and shaking was continued for six days, during which time sampling was carried out at 5000rpm for 10min, 1mL of supernatant was taken as a sample by a pipette, and 1mL of absolute ethanol was supplemented. The obtained supernatant is subjected to ICP test to measure the concentration of silver ions, and the initial release rate of the all-silicon molecular sieve encapsulated nano silver sample in the example 1 is calculated to be about 3.38mg/L/d and is reduced to about 0.47mg/L/d after six days; the initial release rate of the all-silicon molecular sieve encapsulated nano-silver sample of example 2 was about 1.61mg/L/d, and after six days, the release rate was reduced to about 0.225 mg/L/d; the initial release rate of the all-silicon molecular sieve sample loaded with the nano silver by adopting an impregnation method is about 13.33mg/L/d, and the initial release rate is reduced to about 2.50mg/L/d after six days. Therefore, the all-silicon molecular sieve encapsulated nano-silver bactericide prepared by the method has controllable silver ion release rate.
Experimental example 2 Sterilization Effect test
Respectively weighing 0.2g of all-silicon molecular sieve encapsulated nano-silver sample (taking example 1 as an example) and an all-silicon molecular sieve sample loaded with nano-silver by adopting an immersion method into a sterilized 50mL centrifuge tube, adding 20mL of deionized water, shaking for 30 days, then carrying out centrifugal separation on the sample, washing to remove silver ions adsorbed on the surface, drying, weighing 0.05g of the sample, placing the sample into a sterilized 50mL centrifuge tube, adding 5mL of PBS buffer solution, and shaking for 24 hours at 37 ℃ to enable the sample to be fully and fully stirredAfter releasing Ag ions, 0.1mL of E.coli solution was added thereto as an experimental group, and the same operation was performed with a blank PBS buffer solution as a control group. Culturing the sample with the bacteria liquid in a 37 ℃ incubator for 2h, and performing tenfold dilution to obtain a dilution 10-20.1mL of diluted supernatant is respectively taken from the multiplied samples, the diluted supernatant is uniformly coated in a 9cm plastic culture dish filled with a solid culture medium, the culture is carried out for 18h at 37 ℃, and the samples are taken out for counting, so that the sterilization rate of the all-silicon molecular sieve encapsulated nano-silver sample in the example 1 can reach more than 99 percent; and the all-silicon molecular sieve sample loaded with nano silver by adopting an impregnation method loses the sterilization capability. Therefore, the all-silicon molecular sieve encapsulated nano-silver bactericide prepared by the method has higher bactericidal activity.
The embodiments of the present invention have been described in detail, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, and the scope of protection is still within the scope of the invention.
Claims (10)
1. A preparation method of an all-silicon molecular sieve encapsulated nano-silver bactericide is characterized by comprising the following steps:
s1, adding water into the tetrapropyl ammonium hydroxide solution for dilution, adding (3-mercaptopropyl) trimethoxysilane into the solution to prepare a mixed solution, adding a silver nitrate water solution into the mixed solution, and continuously stirring for more than 30 minutes;
s2, adding tetraethyl silicate into the mixed system obtained in the step S1 to obtain silver-silica sol, and aging the silver-silica sol to obtain silver-silica gel;
s3, statically crystallizing the silver-silicon gel obtained in the step S2, roasting at high temperature in the air atmosphere, and reducing at high temperature in the hydrogen atmosphere to finally obtain the all-silicon molecular sieve packaged nano silver bactericide.
2. The method for preparing the all-silicon molecular sieve encapsulated nano-silver bactericide as claimed in claim 1, wherein the temperature of the static crystallization is 90-125 ℃ and the time is 48-144 hours.
3. The preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide as claimed in claim 1, wherein the high-temperature roasting temperature is 300-550 ℃, the time is 1-8 hours, and the heating rate is 0.5-5 ℃/min.
4. The preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide as claimed in claim 1, wherein the temperature of the high-temperature reduction is 250-500 ℃, the time is 2-4 hours, and the temperature rise rate is 0.5-5 ℃/min.
5. The preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide as claimed in claim 1, wherein the aging temperature is 40-90 ℃ and the aging time is 1-2 hours.
6. The method of claim 1, wherein in step S1, the concentration of the tetrapropylammonium hydroxide solution is 25 wt% to 40 wt%, the concentration of the silver nitrate aqueous solution is 0.2 wt% to 0.3 wt%, and water is added to dilute the silver-silica sol obtained in step S2 to obtain a silver-silica sol with a tetrapropylammonium hydroxide concentration of 9.0 wt% to 10.0 wt%, and a silver nitrate concentration of 0.06 wt% to 0.08 wt%.
7. The preparation method of the all-silicon molecular sieve-encapsulated nano-silver bactericide as claimed in claim 1, wherein the molar ratio of tetrapropylammonium hydroxide to tetraethyl silicate is 1: 2-5.
8. The preparation method of the all-silicon molecular sieve-encapsulated nano-silver bactericide as claimed in claim 1, wherein the molar ratio of silver nitrate to (3-mercaptopropyl) trimethoxysilane is 1: 10-40.
9. The preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide as claimed in claim 1, wherein the molar ratio of tetrapropylammonium hydroxide to (3-mercaptopropyl) trimethoxysilane is 1: 0.15-0.25.
10. The all-silicon molecular sieve encapsulated nano-silver bactericide prepared by the preparation method of the all-silicon molecular sieve encapsulated nano-silver bactericide of any one of claims 1 to 8.
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| CN117802790A (en) * | 2024-02-23 | 2024-04-02 | 汕头市镇盛织造实业有限公司 | Soft high-elastic nylon-spandex composite fabric, preparation method thereof and application thereof in underwear |
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| CN117802790A (en) * | 2024-02-23 | 2024-04-02 | 汕头市镇盛织造实业有限公司 | Soft high-elastic nylon-spandex composite fabric, preparation method thereof and application thereof in underwear |
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