CN115322640A - Preparation method of quick-acting antibacterial antiviral protective layer - Google Patents

Preparation method of quick-acting antibacterial antiviral protective layer Download PDF

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CN115322640A
CN115322640A CN202211069317.1A CN202211069317A CN115322640A CN 115322640 A CN115322640 A CN 115322640A CN 202211069317 A CN202211069317 A CN 202211069317A CN 115322640 A CN115322640 A CN 115322640A
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solution
protective layer
quick
antibacterial
antiviral
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楚蕊
李毕忠
李燕新
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Beijing Chamgo Nano Tech Co ltd
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Abstract

The invention belongs to the technical field of antibacterial and antiviral materials, and particularly relates to a preparation method of a quick-acting antibacterial and antiviral protective layer. The preparation method comprises the following steps: uniformly mixing and stirring the double-chain quaternary ammonium salt and the nano silver solution, adding the aqueous solvent, and continuously stirring to obtain a uniform and transparent solution A; then adding organic acid salt into the solution A, continuously stirring at the temperature of 40-50 ℃, and cooling to room temperature to obtain solution B; then adding an aqueous solvent into the solution B, and simultaneously dropwise adding a high-molecular film forming agent into the solution B to obtain a stable and uniform yellowish-white solution C; and wiping or spraying the solution C on the surface of an object, and airing under natural conditions to form the quick-acting antibacterial antiviral protective layer. The antibacterial and antiviral protective layer prepared by the method has the advantages of quick and stable antibacterial and antiviral functions, convenient operation, good effect and the like, and the functions of the antibacterial and antiviral protective layer are integrated, so that the defects of the existing protective layer are overcome, the use is safer, and the personnel infection is avoided.

Description

Preparation method of quick-acting antibacterial antiviral protective layer
Technical Field
The invention belongs to the technical field of antibacterial and antiviral materials, and particularly relates to a preparation method of a quick-acting antibacterial and antiviral protective layer.
Background
The quaternary ammonium salt antibacterial and antiviral material has the advantages of high antibacterial activity, stable and durable performance, low residual toxicity, low irritation to human tissues and the like, and is concerned. The disinfection spray products on the market at present have poor timeliness and odor stimulation, and need to be repeatedly sprayed at intervals, and the conventional disinfection occupies a large amount of manpower and material resources, so that the development of a quick-acting and long-acting disinfection spray can form an antibacterial and antiviral protective film, and is necessary to provide lasting protection. Chinese patent No. cn202010158219.X discloses a protective film formed by nano silver antibacterial spray coating and its preparation method, which is formed by using single inorganic nano silver antibacterial coating, and although it has a certain antibacterial property, it does not reach quick-acting antibacterial and antiviral property, and has requirements for film thickness, resulting in high dosage and high cost. Furthermore, chinese patent CN202010909992.5 discloses a surface antibacterial film and a preparation method thereof, which requires the antibacterial film to be adhered to the surface of an object, and has the problems of inconvenient operation, manpower and material consumption, and adhesion of some special surfaces. Therefore, research and development of a protective layer which is simple in operation, safe, nontoxic and has a quick-acting and stable function are urgently needed.
In view of the above, the invention adopts nano silver as a core, quaternary ammonium salt as a capsule, and combines a polymer film-forming agent, and adopts the positive charge of the quaternary ammonium salt to adsorb bacteria, and the nano silver destroys DNA or RNA genetic materials of the bacteria or viruses, thereby preparing the quick-acting antibacterial antiviral protective layer.
Disclosure of Invention
Aiming at the defects of slow effect taking time, inconvenient operation, incapability of having quick-acting antibacterial and antiviral dual effects and the like of the existing antibacterial protective layer, the invention provides the preparation method of the quick-acting antibacterial and antiviral protective layer, so that the prepared antibacterial and antiviral protective layer has the functions of quick-acting and stable antibacterial and antiviral functions, convenient operation, good effect and the like, the defects of the existing protective layer are overcome, the use is safer, and the personnel infection is avoided.
The invention is realized by the following technical scheme:
the invention provides a preparation method of a quick-acting antibacterial antiviral protective layer, which is characterized by comprising the following steps:
(1) Uniformly stirring the double-chain quaternary ammonium salt and the nano silver solution at the temperature of 60-70 ℃, then adding the aqueous solvent, and continuously stirring to obtain a uniform and transparent solution, which is marked as solution A;
(2) Adding organic acid salt into the solution A obtained in the step (1) under the stirring condition to obtain a transparent solution, continuously stirring for 20-30 min at the temperature of 40-50 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40-50 ℃, adding an aqueous solvent into the solution B under the stirring condition, and simultaneously dropwise adding a high-molecular film-forming agent into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) wiping or spraying the solution C obtained in the step (3) on the surface of an object, and airing under natural conditions to form the quick-acting antibacterial antiviral protective layer.
Preferably, the mass-volume ratio of the double-chain quaternary ammonium salt to the nano silver solution in the step (1) is (0.1-3.0): (5-100) g/mL; the mass-volume ratio of the double-chain quaternary ammonium salt to the aqueous solution is (0.1-3.0): (50-1000) g/mL.
Further, the double-chain quaternary ammonium salt is one or a mixture of more of didodecyldimethylammonium chloride, didodecyldimethylammonium bromide, didodecyldimethylammonium chloride and dioctadecyldimethylammonium chloride.
The invention adopts double-chain quaternary ammonium salt and organic acid salt to carry out ion exchange reaction to form micelle, which is beneficial to the slow release effect of nano silver, and is more stable compared with the micelle formed by common quaternary ammonium salt or chitosan quaternary ammonium salt, and the formed antibacterial and antiviral protective layer has better durability.
Preferably, the concentration of the nano silver solution is 100-1000 ppm, the solvent in the nano silver solution is one or a mixture of distilled water, absolute methanol and absolute ethanol, and the average particle size of the nano silver is 20-30 nm.
Preferably, the mass ratio of the added amount of the organic acid salt to the double-chain quaternary ammonium salt in the step (2) is (0.1-1.0): (0.1-3.0).
Further, the organic acid salt is one or a mixture of more of sodium gluconate, potassium sorbate, sodium benzoate, sodium abietate, sodium oleate, sodium undecyl benzene sulfonate, sodium dodecyl benzene sulfonate, sodium hexadecyl benzene sulfonate, sodium dodecyl sulfate, sodium methyl p-hydroxybenzoate and sodium dodecyl diphenyl ether disulfonate.
Preferably, the mass ratio of the added amount of the high molecular film forming agent to the double-chain quaternary ammonium salt in the step (3) is (0.1-3.0): (0.1-3.0).
Further, the polymer film forming agent is one or a mixture of a plurality of water-soluble polymer acrylate emulsion, water-soluble polyurethane emulsion and polyvinylpyrrolidone.
Preferably, the rotation speed of the stirring in the step (2) is 800-1000 rpm, and the rotation speed of the stirring in the step (3) is 1200-1500 rpm.
Preferably, the aqueous solvent in step (1) and step (3) is one or more of distilled water, anhydrous methanol and anhydrous ethanol.
Compared with the prior art, the invention has the following effects:
(1) The preparation method comprises the steps of carrying out ion exchange reaction on double-chain quaternary ammonium salt and organic acid salt to form micelle, wrapping nano silver to prepare micelle-wrapped nano silver, matching with a high-molecular film-forming agent to prepare a spray which is sprayed on the surface of a solid, and forming a layer of protective film after water is evaporated.
(2) The antibacterial and antiviral protective layer prepared by the invention is wide in application, has quick and efficient virus and bacteria killing effect, is applied to disinfection treatment in public places, and can reduce or avoid the problem of cross infection of personnel to a certain extent. The invention has the advantages of simple and convenient preparation process, high safety, low cost, good effect and the like, and is suitable for industrial large-scale production and application.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. The following description of at least one exemplary embodiment is merely illustrative in nature and is in no way intended to limit the invention, its application, or uses. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Unless specifically stated otherwise, the numerical values set forth in these examples do not limit the scope of the invention. Techniques, methods known to those of ordinary skill in the relevant art may not be discussed in detail, but are intended to be part of the specification where appropriate. In all examples shown and discussed herein, any particular value should be construed as merely illustrative, and not limiting. Thus, other examples of the exemplary embodiments may have different values.
The experimental methods of the following examples, which are not specified under specific conditions, are generally determined according to national standards; if no corresponding national standard exists, the method is carried out according to the universal international standard or the standard requirement proposed by related enterprises. Unless otherwise indicated, all parts are parts by weight and all percentages are percentages by weight.
Example 1
The embodiment provides a preparation method of a quick-acting antibacterial antiviral protective layer, which comprises the following steps:
(1) 0.1g of didodecyldimethylammonium chloride and 10mL of nano-silver aqueous solution with Ag concentration of 1000ppm are stirred uniformly at the temperature of 60 ℃, then 100mL of distilled water is added into the solution, and stirring is continued to obtain uniform and transparent solution, which is marked as solution A;
(2) Adding 0.3g of sodium dodecyl diphenyl ether disulfonate into the solution A obtained in the step (1) under the stirring condition of the rotating speed of 800rpm to obtain a transparent solution, continuously stirring for 30min at the temperature of 40 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40 ℃, adding 50mL of distilled water into the solution B under the stirring condition of the rotation speed of 1200-1500 rpm, and simultaneously dropwise adding 0.5g of water-soluble high-molecular acrylic ester emulsion into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) spraying the antibacterial and antiviral solution C obtained in the step (3) on the surface of PP plastic with the thickness of 5 multiplied by 5cm, and airing under natural conditions to form a quick-acting antibacterial and antiviral protective layer.
Example 2
The embodiment provides a preparation method of a quick-acting antibacterial antiviral protective layer, which comprises the following steps:
(1) Stirring 0.5g of didodecyldimethylammonium chloride and 10mL of nano-silver aqueous solution with Ag concentration of 1000ppm uniformly at 60 ℃, then adding 100mL of distilled water, and continuing stirring to obtain uniform and transparent solution, which is marked as solution A;
(2) Adding 0.3g of sodium dodecyl diphenyl ether disulfonate into the solution A obtained in the step (1) under the stirring condition of the rotating speed of 800rpm to obtain a transparent solution, continuously stirring for 30min at the temperature of 40 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40 ℃, adding 50mL of distilled water into the solution B under the stirring condition of the rotation speed of 1200-1500 rpm, and simultaneously dropwise adding 0.5g of water-soluble high-molecular acrylic ester emulsion into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) spraying the antibacterial and antiviral solution C obtained in the step (3) on the surface of PP plastic with the thickness of 5 multiplied by 5cm, and airing under natural conditions to form a quick-acting antibacterial and antiviral protective layer.
Example 3
The embodiment provides a preparation method of a quick-acting antibacterial antiviral protective layer, which comprises the following steps:
(1) Uniformly stirring 0.25g of didodecyldimethylammonium chloride, 0.25g of didodecyldimethylammonium chloride and 10mL of nano-silver aqueous solution with Ag concentration of 1000ppm at the temperature of 60 ℃, then adding 100mL of distilled water into the solution, and continuously stirring to obtain a uniform and transparent solution, which is marked as solution A;
(2) Adding 0.3g of sodium dodecyl diphenyl ether disulfonate into the solution A obtained in the step (1) under the stirring condition of the rotating speed of 800rpm to obtain a transparent solution, continuously stirring for 30min at the temperature of 40 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40 ℃, adding 50mL of distilled water into the solution B under the stirring condition of the rotation speed of 1200-1500 rpm, and simultaneously dropwise adding 0.5g of water-soluble high-molecular acrylic ester emulsion into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) spraying the antibacterial and antiviral solution C obtained in the step (3) on the surface of PP plastic with the thickness of 5 multiplied by 5cm, and airing under natural conditions to form a quick-acting antibacterial and antiviral protective layer.
Example 4
The embodiment provides a preparation method of a quick-acting antibacterial antiviral protective layer, which comprises the following steps:
(1) Stirring 0.5g of didodecyldimethylammonium chloride and 10mL of nano-silver aqueous solution with Ag concentration of 1000ppm uniformly at 60 ℃, then adding 100mL of distilled water, and continuing stirring to obtain uniform and transparent solution, which is marked as solution A;
(2) Adding 0.5g of sodium dodecyl diphenyl ether disulfonate into the solution A obtained in the step (1) under the stirring condition of the rotating speed of 800rpm to obtain a transparent solution, continuously stirring for 30min at the temperature of 40 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40 ℃, adding 50mL of distilled water into the solution B under the stirring condition of the rotation speed of 1200-1500 rpm, and simultaneously dropwise adding 0.5g of water-soluble high-molecular acrylic ester emulsion into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) spraying the antibacterial and antiviral solution C obtained in the step (3) on the surface of PP plastic with the thickness of 5 multiplied by 5cm, and airing under natural conditions to form a quick-acting antibacterial and antiviral protective layer.
Example 5
The embodiment provides a preparation method of a quick-acting antibacterial antiviral protective layer, which comprises the following steps:
(1) Stirring 0.5g of dioctadecyl dimethyl ammonium chloride and 10mL of nano-silver aqueous solution with Ag concentration of 1000ppm uniformly at the temperature of 60 ℃, then adding 100mL of distilled water, and continuously stirring to obtain a uniform and transparent solution, which is marked as solution A;
(2) Adding 0.5g of sodium methyl p-hydroxybenzoate into the solution A obtained in the step (1) under the stirring condition of the rotation speed of 800rpm to obtain a transparent solution, continuously stirring for 30min at the temperature of 40 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40 ℃, adding 50mL of distilled water into the solution B under the stirring condition of the rotation speed of 1200-1500 rpm, and simultaneously dropwise adding 0.5g of polyvinylpyrrolidone into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) spraying the antibacterial and antiviral solution C obtained in the step (3) on the surface of PP plastic with the thickness of 5 multiplied by 5cm, and airing under natural conditions to form a quick-acting antibacterial and antiviral protective layer.
Comparative examples 1 to 3
The fast-acting antibacterial and antiviral protective layers of comparative examples 1 to 3 were prepared in the same manner as in example 2 except that:
didodecyldimethylammonium chloride was omitted in comparative example 1;
the water-soluble high molecular acrylate emulsion was omitted in comparative example 2;
sodium dodecyl diphenyl oxide disulfonate was omitted from comparative example 3.
The antibacterial and antiviral protective layers prepared in the above examples and comparative examples are measured according to the measurement of the antiviral activity of the international organization for standardization standard ISO 21702-2019 plastic and other non-porous surfaces and the evaluation method of the antibacterial performance of the surfaces of ISO 22196-2011 plastic products, the antiviral performance and the antibacterial performance of the protective layers are tested, and the detection data of examples 1 to 4 and comparative examples 1 to 3 are shown in Table 1.
TABLE 1
Figure RE-GDA0003884523880000081
As is clear from the results of the examination in Table 1, the results in example 1 are inferior, and the results are due to the low content of the double-chain quaternary ammonium salt. In the antiviral and antibacterial protective layers prepared in examples 2 to 5, the higher the amount of the organic acid salt is, the better the micelle-encapsulating effect is, as compared with example 2 and example 4, and the antibacterial and antiviral effect of the protective layer becomes relatively weaker. Comparison among comparative examples 1, 2 and 2 shows that the use of nano silver alone has a poor effect on quick-acting antibacterial and antiviral effects.
The test pieces prepared in comparative example 2, comparative example 3 and example 2 were soaked in water for 24 hours and subjected to a durability test after exposure to natural light for 7 days, and the test results are shown in table 2.
TABLE 2
Figure RE-GDA0003884523880000082
Figure RE-GDA0003884523880000091
As can be seen from table 2, the protective layer formed by the micelle-encapsulated nano silver spray prepared by adding sodium dodecyl diphenyl ether disulfonate and ammonium didodecyldimethylammonium chloride in example 2 under natural conditions has good durability and better antibacterial and antiviral effects under 7-day natural conditions. Comparative example 2 does not contain a polymer film-forming agent, so that the antibacterial material runs off to a certain extent under the aqueous condition, and the lasting effect of the antibacterial and antiviral properties is poor. Comparative example 3 does not contain sodium dodecyl diphenyl ether disulfonate, which causes the loss of the double-chain quaternary ammonium salt in water and leads to the serious decline of the antibacterial and antiviral effects. Therefore, the nano silver wrapped by the micelle has good antibacterial and antiviral effects, and the antibacterial and antiviral functions of the double-chain quaternary ammonium salt and the nano silver are fully exerted. The defects that the effect is poor when single nano silver is used and the durability is poor when double-chain quaternary ammonium salt is used singly in the prior art are overcome.
The above-mentioned embodiments are intended to illustrate the objects, technical solutions and advantages of the present invention in further detail, and it should be understood that the above-mentioned embodiments are only exemplary embodiments of the present invention, and are not intended to limit the present invention, and any modifications, equivalents, improvements and the like made within the spirit and principle of the present invention should be included in the protection scope of the present invention.

Claims (10)

1. A preparation method of a quick-acting antibacterial antiviral protective layer is characterized by comprising the following steps:
(1) Uniformly stirring the double-chain quaternary ammonium salt and the nano silver solution at the temperature of 60-70 ℃, then adding the aqueous solvent, and continuously stirring to obtain a uniform and transparent solution, which is marked as solution A;
(2) Adding organic acid salt into the solution A obtained in the step (1) under the stirring condition to obtain a transparent solution, continuously stirring for 20-30 min at the temperature of 40-50 ℃, and cooling to room temperature to obtain a solution B;
(3) Controlling the temperature to be 40-50 ℃, adding an aqueous solvent into the solution B under the stirring condition, and simultaneously dropwise adding a high-molecular film-forming agent into the solution B to obtain a stable and uniform yellowish white solution C;
(4) And (4) wiping or spraying the solution C obtained in the step (3) on the surface of an object, and airing under natural conditions to form the quick-acting antibacterial antiviral protective layer.
2. The method for preparing a quick-acting antibacterial and antiviral protective layer according to claim 1, wherein the mass-to-volume ratio of the double-chain quaternary ammonium salt to the nano-silver solution in step (1) is (0.1-3.0): (5-100) g/mL; the mass volume ratio of the double-chain quaternary ammonium salt to the aqueous solution is (0.1-3.0): (50-1000) g/mL.
3. The method of claim 2, wherein the double-chain quaternary ammonium salt is one or more of didodecyldimethylammonium chloride, didodecyldimethylammonium bromide, didodecyldimethylammonium chloride, and dioctadecyldimethylammonium chloride.
4. The method for preparing a rapid-acting antibacterial antiviral protective layer according to claim 2, wherein the concentration of the nano silver solution is 100-1000 ppm, the solvent in the nano silver solution is one or more of distilled water, absolute methanol and absolute ethanol, and the average particle size of the nano silver is 20-30 nm.
5. The method for preparing a quick-acting antibacterial and antiviral protective layer according to claim 1, wherein the mass ratio of the added amount of the organic acid salt to the double-chain quaternary ammonium salt in the step (2) is (0.1-1.0) to (0.1-3.0).
6. The method for preparing a rapid-acting antibacterial antiviral protective layer according to claim 5, wherein the organic acid salt is one or more of sodium gluconate, potassium sorbate, sodium benzoate, sodium abietate, sodium oleate, sodium undecyl benzene sulfonate, sodium dodecyl benzene sulfonate, sodium hexadecyl benzene sulfonate, sodium dodecyl sulfate, sodium methyl p-hydroxybenzoate, and sodium dodecyl diphenyl ether disulfonate.
7. The method for preparing a quick-acting antibacterial and antiviral protective layer according to claim 1, wherein the mass ratio of the added amount of the polymeric film-forming agent to the double-chain quaternary ammonium salt in the step (3) is (0.1-3.0): (0.1-3.0).
8. The method for preparing a rapid-acting antibacterial antiviral protective layer according to claim 7, wherein said polymeric film-forming agent is one or a mixture of water-soluble polymeric acrylate emulsion, aqueous polyurethane emulsion and polyvinylpyrrolidone.
9. The method for preparing a quick-acting antibacterial and antiviral protective layer according to claim 1, wherein the rotation speed of the stirring in the step (2) is 800-1000 rpm, and the rotation speed of the stirring in the step (3) is 1200-1500 rpm.
10. The method for preparing a quick-acting antibacterial and antiviral protective layer according to claim 1, wherein the aqueous solvent in step (1) and step (3) is one or more of distilled water, absolute methanol, and absolute ethanol.
CN202211069317.1A 2022-09-02 2022-09-02 Preparation method of quick-acting antibacterial antiviral protective layer Pending CN115322640A (en)

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