CN115584057A - Silane coupling agent modified nano titanium dioxide functionalized nano silver modifier, preparation method thereof and application thereof in resisting viruses in silicone rubber - Google Patents
Silane coupling agent modified nano titanium dioxide functionalized nano silver modifier, preparation method thereof and application thereof in resisting viruses in silicone rubber Download PDFInfo
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Abstract
The invention discloses a silane coupling agent modified nano titanium dioxide functionalized nano silver modifier, a preparation method thereof and an anti-virus application thereof in silicone rubber. The preparation method comprises the following steps: dissolving nano titanium dioxide in ethanol, and sequentially dropwise adding a silane coupling agent, triethylamine, silver nitrate and sodium borohydride in a nitrogen atmosphere to react to obtain the nano titanium dioxide. The nano silver modifier is added into the silicon rubber, has good dispersion phase compatibility, obtains good antiviral performance on the basis of not reducing the physical and mechanical properties of the material, and has good antibacterial property.
Description
Technical Field
The invention relates to the technical field of rubber materials, in particular to a preparation method of a silane coupling agent modified nano titanium dioxide functionalized nano silver modifier and an anti-virus application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in silicone rubber.
Background
Currently, the use of antiviral materials to effectively inhibit and destroy viruses to protect human health is a powerful measure. More antiviral materials are mainly medical masks, and the antiviral materials effectively prevent the virus from being transmitted along with droplets and the like in a physical isolation mode, but cannot meet the requirement of preventing the virus from being transmitted in contact in various occasions of daily life.
The silicone rubber has excellent chemical stability, physiological inertia and biocompatibility, is nontoxic and tasteless, and is widely applied to various aspects of human life such as medical materials, medical instruments, human body wearable materials, articles for daily use and the like. If the silicone rubber has self-antivirus property, the cross infection can be effectively prevented, and the health of human beings is protected. Therefore, the development of novel silicone rubber biological protective materials with high-efficiency antiviral function, which are suitable for various daily life occasions, is urgent.
Nano silver has been known for a long time for its antibacterial action, but due to the small size effect of nano particles, the nano particles have small particle size and high surface activity, and have poor compatibility and poor dispersibility when combined with silicone rubber, and are easy to agglomerate, so that the physical and mechanical properties of the silicone rubber are reduced, the surface treatment of the silicone rubber can reduce the antiviral long-term effect, and in addition, the addition of some silver-series antibacterial agents can also easily influence the vulcanization performance of the silicone rubber. Therefore, effective modification and modification of nano silver particles are urgently needed, the interfacial energy between the nano silver particles and silicon rubber is reduced, the compatibility between the nano silver particles and the silicon rubber is increased, and effective antiviral and antibacterial effects can be achieved on the basis that the vulcanization performance of the material is not influenced and the physical and mechanical properties of the material are not reduced.
Disclosure of Invention
In order to solve the defects and shortcomings of the prior art, the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier, the preparation method thereof and the anti-virus application thereof in silicone rubber are provided.
The purpose of the invention is realized by the following technical scheme:
the invention aims to provide a novel nano-silver modifier for enabling silicone rubber to have an antiviral function, and the nano-silver modifier is prepared from the following raw materials in parts by mass: 0.3 to 3 parts of nano titanium dioxide, 0.5 to 5 parts of silane coupling agent, 0.3 to 3 parts of triethylamine, 0.5 to 2 parts of silver nitrate and 0.2 to 2 parts of sodium borohydride.
Further, the silane coupling agent is 3-mercaptopropyltrimethoxysilane KH590 with a mercapto group.
Further, the silane coupling agent is 3-aminopropyltrimethoxysilane KH540 with an amino group.
The invention also aims to provide a preparation method of the novel nano silver modifier for endowing the silicon rubber with an antiviral function, which comprises the following steps: adding 0.3-3 g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion; dropwise adding a silane coupling agent and triethylamine in a nitrogen atmosphere, and refluxing for 1-3 hours at 40-80 ℃; adding 0.5-2 g of silver nitrate, reacting for 1-2 hours, adding a reducing agent sodium borohydride, and continuing to react for 2-4 hours; and centrifugally washing the obtained solution with ethanol for three times, each time for 5-15 minutes, filtering and drying to obtain the nano-silver modified by the nano-titanium dioxide modified by the silane coupling agent.
The invention also aims to provide the application of the antiviral silicone rubber, and the method has wide raw material sources, and the prepared silicone rubber has good antiviral property and can improve other properties of the rubber, such as antibacterial property and ultraviolet aging resistance.
The antiviral silicone rubber comprises, by mass, 0.5-2.5 parts of vulcanizing agent 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane, 0.5-2.5 parts of bis-dipenta for short, 0.2-2 parts of silane coupling agent modified nano titanium dioxide functionalized nano silver modifier and 100 parts of silicone rubber.
In the application, the silicon rubber is TY971-70 in parts by mass, and the mixing amount is 100 parts by mass.
In the application, the bis-di-penta vulcanizing agent is in a paste form, and the mixing amount is 0.5-2.5 parts by mass.
The application comprises the following steps:
(1) The formula (mass portions) is as follows: weighing 0.5-2.5 parts by mass of pasty bis-penta vulcanizing agent, 0.2-2 parts by mass of nano silver modifier functionalized by modifying nano titanium dioxide with silane coupling agent, and 100 parts by mass of silicone rubber;
(2) Mixing: adding the weighed silicon rubber, the bis-penta vulcanizing agent and the nano silver modifier functionalized by the nano titanium dioxide modified by the silane coupling agent into an open mill for mixing; the feeding and operation sequence is as follows: raw rubber (wrapping roller) → nano silver modifier → turnover → di-v vulcanizing agent → turnover to prepare rubber compound, tabletting through a flat vulcanizing machine, and cooling to prepare the antiviral silicone rubber.
In the above application, the mixing conditions adopted in step (2) are as follows: the mixing period is 10min.
In the application, in the step (2), the feeding and operating sequence is as follows: adding crude rubber, adding a nano silver modifier functionalized by using silane coupling agent and modified nano titanium dioxide, turning, adding a pasty bis-penta vulcanizing agent, turning to prepare rubber, tabletting by using a flat vulcanizing machine, and cooling to obtain the antiviral silicone rubber.
Compared with the prior art, the invention has the following advantages and beneficial effects:
(1) The nano silver modifier prepared by the invention is applied to the silicon rubber, has good dispersion compatibility, does not reduce the vulcanization and physical and mechanical properties of the silicon rubber, and can improve the antiviral property of the silicon rubber.
(2) The antiviral silicone rubber prepared by the invention has antiviral property, good antibacterial property and more excellent ultraviolet aging resistance.
Detailed Description
The invention is explained and illustrated in further detail below with reference to specific examples.
Example 1
A nanometer silver modified by nanometer titanium dioxide modified by silane coupling agent KH-590, the preparation method comprises the following steps:
(1) Adding 0.3g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion;
(2) Dropwise adding 0.8g of 3-mercaptopropyltrimethoxysilane (KH-590) and 0.3g of triethylamine in a nitrogen atmosphere, and refluxing at 60 ℃ for 2 hours;
(3) Adding 1g of silver nitrate, reacting for 2 hours, adding 0.2g of sodium borohydride serving as a reducing agent, and continuing to react for 3 hours;
(4) Centrifuging and washing the obtained solution with ethanol for three times, filtering and drying; namely, the nano titanium dioxide nano silver modifier modified by KH-590 is obtained.
A preparation method of the rubber compound comprises the following steps:
100g of raw rubber is added into an open mill for plastication, the roller spacing is reduced to 5mm at the beginning, and then the raw rubber is gradually enlarged. After the raw rubber coated roller is plastified smoothly and uniformly, 1g of nano-silver modified by KH-590 nano-titanium dioxide is added, the left and right cutters are used for several times, after the nano-silver is uniformly dispersed, 2g of pasty bis-penta vulcanizing agent is added, the left and right cutters are used for several times, and the mixture is rolled for 15 times to obtain a rubber compound, which is marked as SR/TiO2-KH590-Ag-1.
The raw rubber is high transparent gas phase silicon rubber TY971-70.
Example 2
A nanometer silver modified by nanometer titanium dioxide modified by silane coupling agent KH-590, the preparation method comprises the following steps:
(1) Adding 0.3g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion;
(2) Dropwise adding 0.8g of 3-mercaptopropyltrimethoxysilane (KH-590) and 0.3g of triethylamine in a nitrogen atmosphere, and refluxing at 60 ℃ for 2 hours;
(3) Adding 1g of silver nitrate, reacting for 2 hours, adding 0.2g of reducing agent sodium borohydride, and continuing to react for 3 hours;
(4) Centrifuging and washing the obtained solution with ethanol for three times, filtering and drying; namely, the nano titanium dioxide nano silver modifier modified by KH-590 is obtained.
A preparation method of the rubber compound comprises the following steps:
100g of raw rubber is added into an open mill for plastication, the roller spacing is smaller by 5mm at the beginning, and then the raw rubber is gradually enlarged. After the raw rubber coated roller is plasticated smoothly and uniformly, 2g of nano silver modified by the KH-590 modified nano titanium dioxide is added, the left and right cutters are used for several times, after the nano silver is dispersed uniformly, 2g of pasty bis-penta vulcanizing agent is added, the left and right cutters are used for several times, and the mixture is rolled for 15 times to obtain a rubber compound, which is marked as SR/TiO2-KH590-Ag-2.
The raw rubber is high transparent gas phase silicon rubber TY971-70.
Example 3
A nanometer silver modified by nanometer titanium dioxide modified by silane coupling agent KH-540, the preparation method comprises the following steps:
(1) Adding 0.3g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion;
(2) Dropwise adding 0.7g of 3-aminopropyltrimethoxysilane (KH-540) and 0.3g of triethylamine under a nitrogen atmosphere, and refluxing at 60 ℃ for 2 hours;
(3) Adding 1g of silver nitrate, reacting for 2 hours, adding 0.2g of reducing agent sodium borohydride, and continuing to react for 3 hours;
(4) Centrifuging and washing the obtained solution with ethanol for three times, filtering and drying; namely obtaining the nano titanium dioxide nano silver modifier modified by KH-540.
A preparation method of the rubber compound comprises the following steps:
100g of raw rubber is added into an open mill for plastication, the roller spacing is smaller by 5mm at the beginning, and then the raw rubber is gradually enlarged. After the raw rubber roll is plasticated and smooth and uniform, 1g of nano silver modified by the KH-540 modified nano titanium dioxide is added, the left and right cutters are used for several times, 2g of pasty bis-penta vulcanizing agent is added after the raw rubber roll is dispersed uniformly, the left and right cutters are used for several times, and the mixture is rolled for 15 times to obtain a rubber compound, which is marked as SR/TiO2-KH540-Ag.
The raw rubber is high transparent gas phase silicon rubber TY971-70.
Example 4
A nanometer silver modified by nanometer titanium dioxide modified by silane coupling agent KH-540, the preparation method comprises the following steps:
(1) Adding 0.3g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion;
(2) Dropwise adding 0.7g of 3-aminopropyltrimethoxysilane (KH-540) and 0.3g of triethylamine under a nitrogen atmosphere, and refluxing at 60 ℃ for 2 hours;
(3) Adding 1g of silver nitrate, reacting for 2 hours, adding 0.2g of reducing agent sodium borohydride, and continuing to react for 3 hours;
(4) Centrifuging and washing the obtained solution with ethanol for three times, filtering and drying; namely obtaining the nano titanium dioxide nano silver modifier modified by KH-540.
A preparation method of the rubber compound comprises the following steps:
100g of raw rubber is added into an open mill for plastication, the roller spacing is smaller by 5mm at the beginning, and then the raw rubber is gradually enlarged. After the raw rubber coated roller is plastified smoothly and uniformly, 2g of nano silver modified by KH-540 nano titanium dioxide is added, the left and right cutters are used for several times, after the nano silver is uniformly dispersed, 2g of pasty bis-penta vulcanizing agent is added, the left and right cutters are used for several times, and the mixture is rolled for 15 times to obtain a rubber compound, which is marked as SR/TiO2-KH540-Ag.
The raw rubber is high transparent gas phase silicon rubber TY971-70.
Comparative example 1
A preparation method of the rubber compound comprises the following steps:
100g of raw rubber is added into an open mill for plastication, the roller spacing is reduced to 5mm at the beginning, and then the raw rubber is gradually enlarged. After the raw rubber package is plasticated smoothly and uniformly, 2g of pasty bis-penta vulcanizing agent is added, the raw rubber package is cut for several times from left to right, and the raw rubber package is rolled for 15 times to obtain a rubber compound, which is marked as SR.
The crude rubber is high-transparency gas-phase silicone rubber TY971-70.
The difference between the modified nano-silver titanium dioxide modified by KH-590 and the prepared nano-silver titanium dioxide modified by KH-590 is that the modified nano-silver titanium dioxide modified by KH-590 is not added, and the other components, the dosage and the preparation method are the same as those of the modified nano-silver titanium dioxide modified by KH-590 and the prepared nano-silver titanium dioxide modified by KH-590 in the embodiment 1 and the embodiment 2.
The difference between the modified nano-silver titanium dioxide modified with KH-540 and the modified nano-silver titanium dioxide prepared in the method and the embodiments 3 and 4 is that the prepared modified nano-silver titanium dioxide modified nano-silver is not added, and other components, the using amount and the preparation method are the same as those in the embodiments 3 and 4.
And (3) performance testing:
(1) Vulcanization characteristic: testing the vulcanization characteristic of the rubber compound at 170 ℃ by adopting a U-Can UR-2010SD rotor-free vulcanizing instrument;
(2) Tensile strength: testing the tensile strength of the rubber compound by using an UT-2080 tensile testing machine according to a testing method disclosed by GB/T528-2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber;
(3) Tear strength: testing the tearing strength of the rubber compound by using an UT-2080 tensile testing machine according to a testing method disclosed by GB/T528-2009 determination of tensile stress strain performance of vulcanized rubber or thermoplastic rubber;
(4) The antibacterial rate is as follows: according to a determination method disclosed in GB/T31402-2015 plastic surface antibacterial performance experimental method, gram-negative bacteria and gram-positive bacteria are used as test strains to test antibacterial performance;
(5) Plate colony counting test: respectively inoculating gram-negative bacteria and gram-positive bacteria in 75mL broth culture medium, culturing at 150rpm for 24 hr, and diluting to 10 6 、10 5 、 10 4 、10 3 CFU/mL. And putting the sample into a six-hole plate, dripping the diluted bacteria on the surface of the sample, covering the sample with a cover glass, culturing for 24 hours, eluting with a PBS solution, inoculating into a plate culture medium, culturing for 24 hours in a sealed manner, and observing the growth condition of the bacterial colony.
TABLE 1
(6) The antiviral rate: the antiviral performance is tested by taking H1N1 and H3N2 common influenza viruses as test viruses according to ISO 21702-2019 plastic and other non-porous surface antiviral activity tests.
(7) The test method comprises the following steps: all samples were prepared in sterile petri dishes, influenza virus was pipetted onto the surface of the sample to be tested, a thin film was covered to allow the test inoculum to diffuse to the edge without leaking beyond the edge of the thin film, and the samples were incubated at 25 ℃ for 2h up to 24h after sealing. The virus was eluted from the sample with PBS solution, inoculated into 96-well plates and tested for TCID50 ° for calculation of antiviral activity.
TABLE 2
The silane coupling agent modified nano titanium dioxide functionalized nano silver modifier is added to the silicon rubber, so that the vulcanization performance of the silicon rubber is not influenced, the tensile strength, the elongation at break and the tearing strength of the rubber are improved to a certain extent, and the analysis reason is that the addition of the nano silver modifier increases the crosslinking density of the rubber to a certain extent, so that the physical and mechanical properties of the rubber are improved to a certain extent.
As can be seen from tables 1 and 2: with the addition of the nano silver modifier, the antibacterial property of the material is improved, and the material has better antiviral property. In contrast, the inhibition of gram-negative bacteria is superior to the inhibition of gram-positive bacteria. The antibacterial performance of the material is improved due to the fact that the silver ions enhance electron-hole separation on the surface of the nano titanium dioxide, the nano titanium dioxide strong oxidation hydroxyl free radicals and the silver ions are synergistically and continuously released, so that a good inhibition effect is achieved on bacteria, and the hydroxyl and superoxide free radicals with strong oxidation activity generated on the surface of the nano titanium dioxide can effectively inactivate influenza viruses by destroying organic compounds to cause degradation of proteins.
The above examples are illustrative of the present invention, but the embodiments of the present invention are not limited to the above examples, and any other modifications, substitutions, combinations, substitutions of selected materials, additions of auxiliary agents, etc., which are equivalent to the present invention without departing from the principle of the present invention are included in the protection and disclosure of the present invention.
Claims (10)
1. A silane coupling agent modified nano titanium dioxide functionalized nano silver modifier is characterized in that the nano silver modifier is prepared from the following raw materials in parts by mass: 0.3 to 3 parts of nano titanium dioxide, 0.5 to 5 parts of silane coupling agent, 0.3 to 3 parts of triethylamine, 0.5 to 2 parts of silver nitrate and 0.2 to 2 parts of sodium borohydride.
2. The modified nano-silver modified substance with the functionalized nano-titanium dioxide modified by the silane coupling agent as claimed in claim 1, wherein the silane coupling agent is 3-mercaptopropyl trimethoxy silane KH590 with mercapto group.
3. The silane coupling agent modified nano titanium dioxide functionalized nano silver modifier as claimed in claim 1, wherein the silane coupling agent is 3-aminopropyltrimethoxysilane KH540 with amino group.
4. The preparation method of the silane coupling agent modified nanometer titanium dioxide functionalized nanometer silver modifier in any one of the claims 1 to 3 is characterized by comprising the following steps: adding 0.3-3 g of nano titanium dioxide into ethanol, stirring on a magnetic stirrer, and performing ultrasonic dispersion; dropwise adding a silane coupling agent and triethylamine in a nitrogen atmosphere, and refluxing for 1-3 hours at 40-80 ℃; adding 0.5-2 g of silver nitrate, reacting for 1-2 hours, adding a reducing agent sodium borohydride, and continuing to react for 2-4 hours; and (3) centrifugally washing the obtained solution with ethanol for three times, 5-15 minutes each time, filtering and drying to obtain the nano silver modified by the nano titanium dioxide modified by the silane coupling agent.
5. The use of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in the silicone rubber as claimed in any one of claims 1 to 3, wherein the anti-virus silicone rubber comprises, by mass, 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane as a vulcanizing agent, the nano silver modifier functionalized nano titanium dioxide modified by the silane coupling agent, and the silicone rubber.
6. The application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in silicone rubber for resisting viruses as claimed in claim 5, wherein the grade of the silicone rubber is TY971-70, and the mixing amount is 100 parts by mass; the doping amount of the nano silver modifier modified by the silane coupling agent and functionalized by the nano titanium dioxide is 0.2-2 parts by mass.
7. The application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in the silicone rubber for resisting viruses according to claim 5, wherein the vulcanizing agent 2, 5-dimethyl-2, 5-di (tert-butylperoxy) hexane is in the form of paste, and the mixing amount is 0.5-2.5 parts by mass.
8. The application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in silicone rubber for resisting viruses according to claim 5 is characterized by comprising the following steps:
(1) The formula is as follows: weighing 0.5-2.5 parts by mass of pasty bis-penta vulcanizing agent, 0.2-2 parts by mass of nano-silver modifier functionalized by modified nano titanium dioxide with silane coupling agent and 100 parts by mass of silicon rubber;
(2) Mixing: and adding the weighed silicon rubber, the bis-penta vulcanizing agent and the nano silver modifier functionalized by the nano titanium dioxide modified by the silane coupling agent into an open mill for mixing.
9. The application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in silicone rubber for resisting viruses according to claim 8 is characterized in that in the step (2), the mixing conditions are as follows: the mixing period is 10min.
10. The application of the silane coupling agent modified nano titanium dioxide functionalized nano silver modifier in the silicone rubber for resisting viruses according to claim 8 is characterized in that in the step (2), the feeding and operation sequence is as follows: adding a raw rubber wrapping roller, adding a nano silver modifier functionalized by using silane coupling agent modified nano titanium dioxide, turning, adding a pasty bis-penta vulcanizing agent, turning to obtain a rubber compound, tabletting by using a flat vulcanizing machine, and cooling to obtain the antiviral silicone rubber.
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| CN117777733A (en) * | 2023-12-11 | 2024-03-29 | 惠州市港田新材料有限公司 | Antibacterial liquid silica gel and preparation method thereof |
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| CN109337239A (en) * | 2018-09-11 | 2019-02-15 | 浙江西大门新材料股份有限公司 | A kind of preparation method of antibacterial PVC Masterbatch and antibacterial fabric |
| CN109777113A (en) * | 2018-12-07 | 2019-05-21 | 华南理工大学 | A kind of insulating heat-conductive silicon rubber composite material and preparation method thereof |
| CN111019359A (en) * | 2019-12-30 | 2020-04-17 | 广东聚合科技股份有限公司 | High-temperature-resistant antibacterial silicone rubber and preparation method thereof |
| CN113755014A (en) * | 2021-05-26 | 2021-12-07 | 安阳崇高纳米材料科技有限公司 | Antibacterial modified rubber composition and preparation method thereof |
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