CN114015265A - Long-acting antibacterial coating material and preparation method thereof - Google Patents
Long-acting antibacterial coating material and preparation method thereof Download PDFInfo
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- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
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- A—HUMAN NECESSITIES
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- C09D129/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Coating compositions based on hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Coating compositions based on derivatives of such polymers
- C09D129/02—Homopolymers or copolymers of unsaturated alcohols
- C09D129/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
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Abstract
The invention discloses a coating material with long-acting antibiosis, which comprises the following raw materials: 100 parts of polyvinyl alcohol, 0.1-3 parts of ferric oxide micro-nano particles, 500-5000 parts of ultrapure water, 0.25-5 parts of organic antibacterial molecules, 0.1-2 parts of silanized quaternary ammonium salt and 0-3 parts of film forming additives; the particle size of the iron oxide micro-nano particles is 50-1000 nm; the organic antibacterial molecules have coordination groups containing lone pair electrons, and the organic antibacterial molecules are contacted with the iron oxide micro-nano particles to form a coordination effect. The invention also discloses a preparation method of the composition. According to the invention, the long-acting antibacterial performance of the coating is improved through the interaction among the silanized quaternary ammonium salt, the iron oxide micro-nano particles and the organic antibacterial molecules.
Description
Technical Field
The invention relates to the technical field of antibacterial materials, in particular to a coating material with long-acting antibacterial property and a preparation method thereof.
Background
Microorganisms are organisms that are widely found in nature and include fungi, bacteria, viruses, and the like. These ubiquitous microscopic living bodies, invisible to the naked eye, represent the greatest potential hazards of human health and public safety. Some viruses survive on smooth surfaces for long periods of time and spread across the surface of various objects in the living environment, causing the rapid spread of infectious diseases.
As one of the main means for disinfecting the surface of the living environment, various disinfectants such as hypochlorous acid, hydrogen peroxide and the like are used for killing the surface in the whole space, and the method is the most common surface disinfection means at present. In addition, alcohol is also used as a surface disinfectant for small objects. In addition, space sterilization using ultraviolet rays is also one of the commonly used sterilization means. However, disinfectants represented by strong oxidation such as hypochlorous acid and hydrogen peroxide and disinfectants with strong volatility such as alcohol have short action time and little residue, and can not realize the function of permanent killing although the disinfectant is quick, efficient and low in cost. The disinfection and sterilization treatment by using ultraviolet rays is dangerous, and if the ultraviolet lamp is forgotten to be turned off in the daytime, the people in the environment can be greatly injured. Thus, there is currently no viable solution for long-term sterilization. However, in certain crowded places and areas, surfaces without long-lasting antimicrobial sterilization capability are easily and quickly become a route of transmission after disinfection. Therefore, a novel coating with bactericidal effect and long-acting bacteriostasis is developed, so that public health and safety are protected to the maximum extent, environmental pollution is reduced, and the coating has important economic value and significance.
PVA (polyvinyl alcohol) is used as a non-toxic and harmless film forming agent with good biocompatibility, and is widely applied to various industries, such as cosmetics, biomedicine, electronic components, filter materials and the like. The PVA monomer contains hydroxyl group and can form hydrogen bond with water, so that the PVA monomer is a high molecular polymer which can be dissolved in water, and great advantage is brought to the use of PVA. The PVA and the antibacterial component are mixed in the aqueous solution and then coated, so that an antibacterial film can be formed on the surface of the product. However, PVA has excellent water solubility, and is easy to dissolve or swell by water during use, and the antibacterial film layer is easy to rapidly run off during actual use, so that the PVA is ineffective. Therefore, how to balance the water solubility of PVA and the water solubility after film formation is a problem to be solved.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a coating material with long-acting antibacterial property and a preparation method thereof.
In order to achieve the above purpose, the technical scheme of the invention is as follows:
a coating material with long-acting antibacterial function comprises the following raw materials in percentage by weight: 100 parts of polyvinyl alcohol, 500-5000 parts of ultrapure water, 0.1-3 parts of iron oxide micro-nano particles, 0.25-5 parts of organic antibacterial molecules, 0.1-2 parts of silanized quaternary ammonium salt and 0-3 parts of film forming additives; the particle size of the iron oxide micro-nano particles is 50-1000 nm; the organic antibacterial molecules have coordination groups containing lone pair electrons, and the organic antibacterial molecules are contacted with the iron oxide micro-nano particles to form a coordination effect.
Optionally, the alcoholysis degree of the polyvinyl alcohol is 90-99.9%, and the polymerization degree is 1700-1900.
Optionally, the organic antimicrobial molecule comprises at least one of octenidine, polyhexamethylene biguanide, and polyhexamethylene guanidine.
Optionally, the weight ratio of the iron oxide micro-nano particles to the organic antibacterial molecules is 1: 1 to 10.
Optionally, the particle size of the iron oxide micro-nano particles is 100-500 nm.
Optionally, the film-forming additive is a silane-based compound.
A preparation method of the coating material with long-acting antibiosis comprises the following steps:
1) according to the proportion, 100 parts by weight of polyvinyl alcohol is stirred and dissolved in 500-5000 parts by weight of ultrapure water with the temperature higher than 90 ℃, and then the ultrapure water is cooled to room temperature;
2) adding 0.1-3 parts by weight of iron oxide micro-nano particles, and stirring to uniformly disperse the iron oxide micro-nano particles in the sol;
3) adding 0.1-2 parts by weight of silanized quaternary ammonium salt, and fully stirring for dissolving;
4) adding 0.25-5 parts by weight of organic antibacterial molecules, ultrasonically stirring for 12-36 hours, and mixing, wherein the organic antibacterial molecules are contacted with the iron oxide micro-nano particles to form a coordination effect;
5) and adding 0-3 parts by weight of film forming additive, uniformly mixing, coating on the surface of an object, and drying to form the long-acting antibacterial coating.
Optionally, the thickness of the coating is 0.1-10 microns.
Optionally, in the step 5), the coating is performed by spraying a single-fluid spray gun on the surface of the object, wherein the spraying amount is 0.05-0.5L/m2。
Optionally, in step 1), 100 parts by weight of polyvinyl alcohol is dissolved in 800-2000 parts by weight of ultrapure water at a temperature higher than 90 ℃ by stirring, and then cooled to room temperature.
The invention has the beneficial effects that:
the silanized quaternary ammonium salt and PVA are subjected to dehydration condensation to form a net structure, so that the water resistance is improved, the coating film is prevented from being rapidly damaged in daily use, and the structure is more stable; on the other hand, the antibacterial performance of the PVA film brings long-acting antibacterial capability to the PVA film;
the iron oxide micro-nano particles are crosslinked with PVA and silanized quaternary ammonium salt, so that the water resistance is further improved; on the other hand, organic antibacterial molecules capable of coordinating with ferric oxide are introduced, so that the effect of fixing the organic antibacterial molecules in the PVA film is achieved, and the antibacterial performance of the film is improved;
the effect of combining antibiosis and sterilization is achieved through the interaction and combination of the components.
Detailed Description
The following specific examples further illustrate the invention.
A coating material with long-acting antibacterial function comprises the following raw materials in percentage by weight: 100 parts of polyvinyl alcohol, 500-5000 parts of ultrapure water, 0.1-3 parts of iron oxide micro-nano particles, 0.25-5 parts of organic antibacterial molecules, 0.1-2 parts of silanized quaternary ammonium salt and 0-3 parts of film forming additives.
The alcoholysis degree of the PVA is 90-99.9%, preferably 95-99.9%, and the polymerization degree is 1700-1900.
The particle size range of the iron oxide micro-nano particles is 50-1000 nm, preferably 100-500 nm. The ferric oxide micro-nano particles are mainly ferric oxide, wherein ferric ions account for more than 90% of the concentration of all ferric ions.
The organic antibacterial molecule should contain groups with related coordination ligands, such as oxygen lone pair (hydroxyl, sulfhydryl, etc.) and nitrogen lone pair (amine, amide, etc.). The coordination group contains lone pair electrons and can be matched with Fe with empty d electron orbit3+The metal centers are coordinately bound. Organic antimicrobial molecules include, but are not limited to, one or more of octenidine, polyhexamethylene biguanide, polyhexamethylene guanidine, and the like. As an important component of a new generation of broad-spectrum sterilization, organic antibacterial molecules can be combined with microbial cell membranes, cell walls and virus capsids with negative charges through intramolecular positive charge groups, so that the effect of broad-spectrum sterilization of bacteria and viruses is achieved. Because the action mechanism of the antibacterial agent is not specific to a certain biological process, the antibacterial agent cannot generate the drug resistance of bacteria to cause failure in the long-term use process through the organic antibacterial molecules with the positive charge groups.
In order to improve the adhesion strength of the formed antibacterial coating to the surface of the object, a film-forming additive may be added, and the film-forming additive may be a silane-based compound, such as silok 8333.
The preparation method of the coating material with long-acting antibiosis comprises the following steps:
1) according to the proportion, 100 parts by weight of polyvinyl alcohol is stirred and dissolved in 500-5000 parts by weight of ultrapure water with the temperature higher than 90 ℃, and then the ultrapure water is cooled to room temperature; more preferably, the amount of the ultrapure water is 500 to 2000 parts by weight;
2) adding 0.1-3 parts by weight of iron oxide micro-nano particles, and stirring to uniformly disperse the iron oxide micro-nano particles in the sol;
3) adding 0.1-2 parts by weight of silanized quaternary ammonium salt, and fully stirring for dissolving;
4) adding 0.25-5 parts by weight of organic antibacterial molecules, ultrasonically stirring for 12-36 hours, and mixing, wherein the organic antibacterial molecules are contacted with the iron oxide micro-nano particles to form a coordination effect;
5) and adding 0-3 parts by weight of film forming additive, uniformly mixing, coating on the surface of an object, and drying to form the long-acting antibacterial coating.
The coating layer may be formed by, but not limited to, dip coating, spin coating, spray coating, or other film forming methods. Among them, the spraying is simple to use, the film forming is rapid, and the method is not limited by the surface shape of the object and is the most ideal mode. The spraying process adopted by the invention is to spray a single-fluid spray gun on the surface of an object, wherein the spraying amount is 0.05-0.5L/m2. Thereby forming a coating on the surface of the object. The thickness of the coating is about 0.1 to 10 microns.
In the process of spraying, curing and film forming of the spray, silicon oxygen bonds of the silanized quaternary ammonium salt are hydrolyzed and condensed with hydroxyl groups of PVA molecular chains, so that the PVA chains are driven to form a net structure, the crosslinking degree among the PVA high molecular chains is improved, on one hand, the antibacterial capability is brought to the PVA film, on the other hand, the water resistance is increased, and the generated coating film is prevented from being rapidly damaged in daily use; meanwhile, hydroxyl generated on the surface of the iron oxide micro-nano particles can be subjected to crosslinking or dehydration condensation with hydroxyl groups of a PVA chain and silicon-oxygen bonds of a crosslinking antibacterial agent, so that the water resistance of the PVA film is further improved, on the other hand, ferric ions on the surface of the iron oxide nano particles can generate a coordination effect with organic antibacterial molecules, and the antibacterial capability of the PVA antibacterial layer can be effectively improved by introducing the organic antibacterial molecules. Wherein the weight ratio of the ferric oxide micro-nano particles to the organic antibacterial molecules is 1: (1-10).
Therefore, the introduction of the organic silicon quaternary ammonium salt and the organic antibacterial molecules can provide antibacterial capability for the spray coating. The iron oxide micro-nano particles and the organic silicon quaternary ammonium salt can adjust the water resistance of the PVA layer and improve the long-acting property of the coating. The nano iron oxide can anchor antibacterial molecules in the PVA layer, and the antibacterial efficiency and the durability are maximized. The film forming additive can improve the adhesion strength of the coating film and improve the firmness of the coating film. In addition, the quaternary ammonium silicone salts can also provide better surface adhesion and increase durability. The obtained coating has stronger stability and can keep the antibacterial performance for a long time.
In the examples disclosed below, Quaternary silicone salt PC-9911 was obtained from Sesbania silicone; octenidine hydrochloride was purchased from wuhananabai chemical; the rest chemical reagents are general commercial products.
Example 1
For 100 parts by weight of polyvinyl alcohol, 1000 parts by weight of 18 megaohm ultrapure water was heated to 90 ℃ or higher, polyvinyl alcohol (alcoholysis degree of about 90%, polymerization degree of about 1800) was dissolved in the ultrapure water with stirring, the temperature was maintained, stirring was carried out for 2 hours until homogeneity was reached, and cooling was carried out to room temperature. And then adding 1 part by weight of iron oxide micro-nano particles (20-200 nm), stirring for 1 hour, and uniformly mixing. Subsequently, 2 parts by weight of PC-9911, an antibacterial crosslinking agent, was added to the mixture, and the mixture was sufficiently stirred for 10min to dissolve. And then, adding 1 part by weight of octenidine hydrochloride, and dissolving by ultrasonic treatment for 12-36 hours to obtain a mixed solution. The mixed solution is evenly shaken before spraying, and then the mixed solution is coated on the surface of a plastic culture dish by a single-fluid spray gun, wherein the spraying density is about 0.1L/m2And naturally drying to form the long-acting antibacterial coating, wherein the thickness of the coating is about 10 mu m.
Example 2
For 100 parts by weight of polyvinyl alcohol, 1500 parts by weight of 18 megaohm ultrapure water was heated to 90 ℃ or higher, and polyvinyl alcohol (alcoholysis degree of about 90%, polymerization degree of about 1800) was dissolved in the ultrapure water with stirring, and stirred for 2 hours to be uniform while maintaining the temperature, and then cooled to room temperature. Then, 1 part by weight of iron oxide nanoparticles (20 to 200nm) was added, stirred for 1 hour and mixed uniformly. Subsequently, 2 parts by weight of PC-9911, an antibacterial crosslinking agent, was added to the mixture, and the mixture was sufficiently stirred for 10min to dissolve. Then, 1.5 parts by weight of octenidine hydrochloride is added, and the mixture is dissolved by ultrasonic for 12-36 hours to obtain a mixed solutionAnd (4) liquid. The mixed solution is evenly shaken before spraying, and then the mixed solution is coated on the surface of a plastic culture dish by a single-fluid spray gun, wherein the spraying density is about 0.1L/m2And naturally drying to form the long-acting antibacterial coating, wherein the thickness of the coating is about 10 mu m.
Comparative example 1
For 100 parts by weight of polyvinyl alcohol, 1000 parts by weight of 18 megaohm ultrapure water was heated to 90 ℃ or higher, polyvinyl alcohol (alcoholysis degree of about 90%, polymerization degree of about 1800) was dissolved in the ultrapure water with stirring, the temperature was maintained, stirring was carried out for 2 hours until homogeneity was reached, and cooling was carried out to room temperature. The mixed solution is evenly shaken before spraying, and then the mixed solution is coated on the surface of a plastic culture dish by a single-fluid spray gun, wherein the spraying density is about 0.1L/m2And naturally dried to a coating thickness of about 10 μm.
Comparative example 2
For 100 parts by weight of polyvinyl alcohol, 1000 parts by weight of 18 megaohm ultrapure water was heated to 90 ℃ or higher, polyvinyl alcohol (alcoholysis degree of about 90%, polymerization degree of about 1800) was dissolved in the ultrapure water with stirring, the temperature was maintained, stirring was carried out for 2 hours until homogeneity was reached, and cooling was carried out to room temperature. And then, adding 1 part by weight of octenidine hydrochloride, and dissolving by ultrasonic treatment for 12-36 hours to obtain a mixed solution. Shaking before spraying, coating the mixed solution on the surface of a plastic culture dish by using a single-fluid spray gun, and naturally drying to obtain a spray density of about 0.1L/m2The coating thickness was about 10 μm.
To verify the long-term efficacy, we soaked example 1, comparative example 1 and comparative example 2 in ultrapure water for 24h and performed a surface antimicrobial test.
The antibacterial test method comprises the following steps:
3ml of staphylococcus aureus liquid is dripped on the surface of the culture dish sprayed with the PVA antibacterial layer, and the culture dish is incubated for 24 times. Shaking up, sucking 100 microliter of the bacterial liquid into a 96-well plate, and measuring the OD value. The results are as follows:
it can be seen that the examples all showed excellent antibacterial ability. Comparative example 1 had no antibacterial ability because no antibacterial ingredient was added. Comparative example 2 also shows antibacterial ability due to the addition of octenidine organic antibacterial molecule. However, after 24 hours of soaking, since comparative example 2 was not treated to make any PVA water-resistant and, at the same time, octenidine was not anchored in the PVA layer by iron oxide, the soaked comparative example 2 lost the antibacterial ability, and, correspondingly, example 1 after 24 hours of soaking still maintained good antibacterial ability.
The above examples are only intended to further illustrate the long-lasting antibacterial coating material and the preparation method thereof, but the present invention is not limited to the examples, and any simple modification, equivalent change and modification made to the above examples according to the technical spirit of the present invention fall within the scope of the technical solution of the present invention.
Claims (10)
1. A coating material with long-acting antibacterial property is characterized in that the coating material comprises the following raw materials in proportion: 100 parts of polyvinyl alcohol, 500-5000 parts of ultrapure water, 0.1-3 parts of iron oxide micro-nano particles, 0.25-5 parts of organic antibacterial molecules, 0.1-2 parts of silanized quaternary ammonium salt and 0-3 parts of film forming additives; the particle size of the iron oxide micro-nano particles is 50-1000 nm; the organic antibacterial molecules have coordination groups containing lone pair electrons, and the organic antibacterial molecules are contacted with the iron oxide micro-nano particles to form a coordination effect.
2. The coating material having a long-lasting antibacterial property according to claim 1, characterized in that: the alcoholysis degree of the polyvinyl alcohol is 90-99.9%, and the polymerization degree is 1700-1900.
3. The coating material having a long-lasting antibacterial property according to claim 1, characterized in that: the organic antibacterial molecule comprises at least one of octenidine, polyhexamethylene biguanide and polyhexamethylene guanidine.
4. The coating material having a long-lasting antibacterial property according to claim 1, characterized in that: the weight ratio of the iron oxide micro-nano particles to the organic antibacterial molecules is 1: 1 to 10.
5. The coating material having a long-lasting antibacterial property according to claim 1, characterized in that: the particle size of the iron oxide micro-nano particles is 100-500 nm.
6. The coating material having a long-lasting antibacterial property according to claim 1, characterized in that: the film-forming additive is a silane compound.
7. A method for preparing a coating material with long-acting antibacterial function according to any one of claims 1 to 6, which is characterized by comprising the following steps:
1) according to the proportion, 100 parts by weight of polyvinyl alcohol is stirred and dissolved in 500-5000 parts by weight of ultrapure water with the temperature higher than 90 ℃, and then the ultrapure water is cooled to room temperature;
2) adding 0.1-3 parts by weight of iron oxide micro-nano particles, and stirring to uniformly disperse the iron oxide micro-nano particles in the sol
Performing the following steps;
3) adding 0.1-2 parts by weight of silanized quaternary ammonium salt, and fully stirring for dissolving;
4) adding 0.25-5 parts by weight of organic antibacterial molecules, and ultrasonically stirring for 12-36 hours for mixing
The organic antibacterial molecules are contacted with the ferric oxide micro-nano particles to form a coordination effect;
5) adding 0-3 parts by weight of film forming additive, uniformly mixing, coating on the surface of an object, and drying to form the long glass fiber
An antibacterial coating.
8. The method of claim 7, wherein: the thickness of the coating is 0.1-10 microns.
9. The method of claim 7, wherein: in the step 5), the coating is performed by adopting single fluid sprayingThe gun is sprayed on the surface of an object, and the spraying amount is 0.05-0.5L/m2。
10. The method of claim 7, wherein: in the step 1), according to the proportion, 100 parts by weight of polyvinyl alcohol is stirred and dissolved in 800-2000 parts by weight of ultrapure water with the temperature higher than 90 ℃, and then the ultrapure water is cooled to room temperature.
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| CN115581817A (en) * | 2022-09-16 | 2023-01-10 | 南京神奇科技开发有限公司 | Biomedical coating material with antibacterial and lubricating functions and preparation method thereof |
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| CN114685869A (en) * | 2022-03-16 | 2022-07-01 | 厦门赋源高科技有限公司 | Preparation method of antibacterial nitrile butadiene rubber based on surface rapid crosslinking and curing |
| CN115581817A (en) * | 2022-09-16 | 2023-01-10 | 南京神奇科技开发有限公司 | Biomedical coating material with antibacterial and lubricating functions and preparation method thereof |
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