CN114133858A - Preparation method of ordered multi-stage micro-nano structure antibacterial coating - Google Patents
Preparation method of ordered multi-stage micro-nano structure antibacterial coating Download PDFInfo
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- CN114133858A CN114133858A CN202111505734.1A CN202111505734A CN114133858A CN 114133858 A CN114133858 A CN 114133858A CN 202111505734 A CN202111505734 A CN 202111505734A CN 114133858 A CN114133858 A CN 114133858A
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
- C09D175/14—Polyurethanes having carbon-to-carbon unsaturated bonds
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D3/00—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials
- B05D3/02—Pretreatment of surfaces to which liquids or other fluent materials are to be applied; After-treatment of applied coatings, e.g. intermediate treating of an applied coating preparatory to subsequent applications of liquids or other fluent materials by baking
- B05D3/0254—After-treatment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D5/00—Processes for applying liquids or other fluent materials to surfaces to obtain special surface effects, finishes or structures
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B05—SPRAYING OR ATOMISING IN GENERAL; APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D—PROCESSES FOR APPLYING FLUENT MATERIALS TO SURFACES, IN GENERAL
- B05D7/00—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials
- B05D7/24—Processes, other than flocking, specially adapted for applying liquids or other fluent materials to particular surfaces or for applying particular liquids or other fluent materials for applying particular liquids or other fluent materials
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/16—Antifouling paints; Underwater paints
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D7/00—Features of coating compositions, not provided for in group C09D5/00; Processes for incorporating ingredients in coating compositions
- C09D7/20—Diluents or solvents
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Abstract
The invention discloses a preparation method of an ordered multi-stage micro-nano structure antibacterial coating, and relates to a preparation method of an antibacterial coating. The invention aims to solve the technical problems that the method for preparing the micro-nano structure antibacterial coating is complicated, large-area forming cannot be realized, and the preparation on the surface with a complex shape is difficult in the prior art. The preparation method comprises the following steps: mixing polyurethane and epoxy resin, and adding a polar solvent until the polyurethane and the epoxy resin are completely dissolved to obtain a solution A; adding the curing agent into the same polar solvent until the curing agent is completely dissolved to obtain a solution B; mixing the solution A and the solution B, filtering, standing, taking out, and coating on the surface of the component to be protected; and then moving the coating into an oven for annealing, and then crosslinking and curing to obtain the ordered multi-stage micro-nano structure antibacterial coating. The antibacterial coating obtained by the invention has simple preparation process and easily obtained raw materials, and can be used in the fields of cleaning, water prevention, pollution prevention, ice prevention, antibiosis and the like.
Description
Technical Field
The invention relates to a preparation method of an antibacterial coating.
Background
In the marine environment, bacteria, algae and invertebrates are adsorbed to the surface of a material to form a biofilm substrate, and the biofilm substrate provides a living environment for larval marine organisms (such as macroalgae, sponges, barnacles and the like) to propagate on the surface to form a large-area fouling organism community, so that a ship body is rough, the fluid resistance is increased, the operation speed is further reduced, and the oil consumption is increased. The surface of the ship body is coated with a layer of antibacterial antifouling coating, for example, the surface of the ship body is coated with a self-polishing antifouling coating, so that the formation of fouling biological communities on the surface of the ship body can be greatly reduced, but the fouling biological communities are easy to fall off through seawater erosion, and the life cycle is short. The method for preparing the micro-nano structure antibacterial coating by utilizing a template method, a laser etching method and the like has the advantages of complex preparation process, high manufacturing cost due to the need of high-precision instruments and equipment, poor wear resistance of the prepared coating, weak combination with a base material, and great difficulty in manufacturing irregular curved surfaces and surfaces of complex structures in large areas.
Disclosure of Invention
The invention provides a preparation method of an ordered multi-stage micro-nano structure antibacterial coating, aiming at solving the technical problems that the preparation method of the micro-nano structure antibacterial coating in the prior art is complicated, cannot be formed in a large area and is difficult to prepare on the surface with a complex shape.
The invention discloses a preparation method of an ordered multi-level micro-nano structure antibacterial coating, which comprises the following steps:
firstly, respectively weighing 60-90 parts of polyurethane, 10-40 parts of epoxy resin and 5-10 parts of solvent according to the mass part ratio; adding polyurethane and epoxy resin into a reaction container provided with a vacuum stirring system, uniformly mixing, adding a solvent, and mixing for 2-4 hours to completely dissolve the polyurethane and the epoxy resin until the polyurethane and the epoxy resin are clear and transparent to obtain a solution A; wherein the solvent is a medium polar solvent;
respectively weighing 20-30 parts of curing agent and 10-25 parts of solvent according to the mass part ratio; uniformly mixing a curing agent and a solvent to obtain a solution B; wherein the solvent is a medium polar solvent, and is the same as the solvent in the first step;
thirdly, uniformly mixing the solution A and the solution B, filtering by using a screen, standing at room temperature, and coating the mixture on the surface of the component to be protected;
fourthly, moving the component coated on the surface in the third step into an oven with the temperature of 50-60 ℃ for maintaining for 2-3 hours for annealing, raising the temperature to 80-90 ℃ for maintaining for 24-28 hours for crosslinking and curing, and obtaining the ordered multistage micro-nano structure antibacterial coating.
More specifically, the polyurethane in the first step is polybutadiene polyurethane (HTPB-PU).
More recently, the polybutadiene polyurethane (HTPB-PU) has a content of-NCO% of 4% to 6%.
More specifically, the epoxy resin in the first step is bisphenol a type epoxy resin, and the type is E51 or E44.
More further, the solvent in the first step is toluene, benzene, xylene, ketones, esters, ethers or thiols.
More recently, the ester solvent is ethyl acetate.
Further, the curing agent in the second step is 3,3 '-dichloro-4, 4' -diaminodiphenylmethane (MOCA) or diethyltoluenediamine (DETDA).
Furthermore, the mixing ratio of the solution A and the solution B in the third step is (1.2-1.5): 1.
furthermore, the screen mesh in the third step is 200-300 meshes.
Furthermore, the standing time in step three is 30-40 min.
Furthermore, the painting mode in the third step is brushing, dipping, rolling or spraying.
According to the invention, hydroxyl-terminated polybutadiene polyurethane and epoxy resin are blended, different substances have different solubilities in common medium solvents, in the annealing process, epoxy groups and urethane groups with good solubility form an outer shell, polybutadiene with general solubility is gathered to form an inner core, and then the outer shell is crosslinked, cured and self-assembled to obtain a hill-shaped micro-protrusion structure with a regularly arranged surface, and the physical and chemical characteristics and the appearance size of a micro-phase separation structure are adjusted by different molar ratios of soft and hard polyurethane sections, so that a low-surface-energy coating with excellent performances such as hydrophobicity, antifouling property, antibacterial property and the like can be formed.
Compared with a self-polishing coating with a smooth surface, the polyurethane low-surface-energy coating has a longer life cycle, can be continuously used after being impacted by water flow, has good protein adsorption resistance due to the microphase separation structure of the polyurethane, can inhibit the attachment of fouling organisms when being applied to a marine environment, and can effectively prevent the initial adhesion and colonization of bacteria on the surface of a material and the formation of a biological film.
The size of the micro-nano structure can be regulated and controlled by regulating the content of soft and hard segments in a system, the low surface energy performance can be regulated and controlled at the same time, the coating has certain hydrophobicity by regulating and controlling the size of the microstructure, the static water contact angle of the coating is obviously increased compared with that of pure PU (polyurethane) and pure EP (EP) coatings, and the static water contact angle of the coating is obviously improved after the coating is rubbed by 200-mesh abrasive paper, so that the coating has certain wear resistance.
The polyurethane and the epoxy resin adopted by the invention have no silicon or fluorine, the raw materials are easy to obtain, the process is simple, the regular micro-nano structure can be obtained in a large area and at low cost, and the preparation can be carried out on the surface with a complex shape. The low surface energy coating with the regular micro-nano structure has potential application prospect in the fields of self-cleaning, water resistance, pollution resistance, ice resistance, antibiosis and the like in the industries of petroleum, chemical engineering, ships, bridges, buildings and the like.
Drawings
Fig. 1 is a super-depth-of-field three-dimensional topography of the ordered micro-nano structure antibacterial coating prepared in example 1.
Fig. 2 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in example 1.
Fig. 3 is a comparison graph of escherichia coli and staphylococcus aureus resistance of the ordered micro-nano structure antibacterial coating prepared in example 1.
Fig. 4 is a super-depth-of-field three-dimensional topography of the ordered micro-nano structure antibacterial coating prepared in example 2.
Fig. 5 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in example 2.
Fig. 6 is a super-depth-of-field three-dimensional topography of the ordered micro-nano structure antibacterial coating prepared in example 3.
Fig. 7 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in example 3.
Detailed Description
The following examples are used to demonstrate the beneficial effects of the present invention.
Example 1: the preparation method of the ordered multistage micro-nano structure antibacterial coating comprises the following steps:
respectively weighing 90 parts of polybutadiene polyurethane, 10 parts of epoxy resin E51 and 10 parts of toluene according to the mass part ratio; adding polybutadiene polyurethane and epoxy resin E51 into a reaction vessel provided with a vacuum stirring system, uniformly mixing, adding toluene, mixing for 2.5 hours, and completely dissolving the polybutadiene polyurethane and the epoxy resin E51 until the mixture is clear and transparent to obtain solution A; wherein the polybutadiene polyurethane has a-NCO% content of 5%;
respectively weighing 24 parts of diethyl toluene diamine (DETDA) and 25 parts of toluene according to the mass part ratio; uniformly mixing diethyl toluenediamine (DETDA) and toluene to obtain a solution B;
thirdly, uniformly mixing the solution A and the solution B obtained in the second step according to the ratio of 1:1, filtering by a 200-mesh screen, standing for 30min at room temperature, and brushing on a sample plate;
fourthly, the sample plate in the third step is moved into an oven to be annealed for 2 hours at 50 ℃, and then is taken out after being crosslinked and cured for 24 hours at 80 ℃, thus obtaining the antibacterial coating with the highly ordered regular micro-nano structure on the surface.
Fig. 1 is a super-depth-of-field three-dimensional topography of the ordered micro-nano structure antibacterial coating prepared in the embodiment. As can be seen from FIG. 1, the antibacterial coating is highly ordered, and the surface microstructure has a protrusion pitch of 40um (X direction), 50um (Y direction) and a height of 11.96um (Z direction).
Fig. 2 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in the embodiment. As can be seen from fig. 2, the static water contact angle is 102 °, which is a hydrophobic coating. After being rubbed by 200-mesh sandpaper, the contact angle of the ordered micro-nano structure antibacterial coating prepared by the embodiment is improved to 117 degrees, and the coating has hydrophobicity and certain wear resistance.
Escherichia coli and Staphylococcus aureus were selected, and the antibacterial coating prepared in this example was used for an antibacterial test, which was measured with reference to GB/T21510 film-sticking method. Fig. 3 is a comparison graph (a-escherichia coli, b-staphylococcus aureus) of the ordered micro-nano structure antibacterial coating prepared in the embodiment, and it can be seen from the comparison experiment graph that the antibacterial rates of the coating prepared in the embodiment to escherichia coli and staphylococcus aureus are 93.66% and 100%, respectively. The coating prepared in the embodiment has the advantages that the hard polyurethane segment content is 44.6% and the epoxy resin content is 30% through calculation, and the coating has a micro-nano structure which is formed by self-assembling the polyurethane and the epoxy resin in a solvent through chemical bonds, hydrogen bonds, a click chemical action of olefin and a special micro-phase separation structure formed by the polyurethane and the epoxy resin, has high orderly regularity, can resist the adsorption of escherichia coli and staphylococcus aureus, achieves the sterilization effect and has high-efficiency antibacterial property.
Example 2: the preparation method of the ordered multistage micro-nano structure antibacterial coating comprises the following steps:
respectively weighing 80 parts of polybutadiene polyurethane, 24 parts of epoxy resin E51 and 8 parts of toluene according to the mass part ratio; adding polybutadiene polyurethane and epoxy resin E51 into a reaction vessel provided with a vacuum stirring system, uniformly mixing, adding toluene, and mixing for 3 hours to completely dissolve the polybutadiene polyurethane and the epoxy resin E51 until the mixture is clear and transparent, so as to obtain a solution A; wherein the polybutadiene polyurethane has a-NCO% content of 5%;
respectively weighing 22 parts of diethyl toluene diamine (DETDA) and 16 parts of toluene according to the mass part ratio; uniformly mixing diethyl toluenediamine (DETDA) and toluene to obtain a solution B;
thirdly, uniformly mixing the solution A and the solution B obtained in the second step according to the ratio of 1:1, filtering by a 200-mesh screen, standing for 30min at room temperature, and brushing on a sample plate;
fourthly, the sample plate in the third step is moved into an oven to be annealed for 2 hours at 50 ℃, and then is taken out after being crosslinked and cured for 24 hours at 80 ℃, thus obtaining the antibacterial coating with the highly ordered regular micro-nano structure on the surface.
Fig. 4 is a super-depth-of-field three-dimensional topography picture of the ordered micro-nano structure antibacterial coating prepared in the embodiment. It can be seen from fig. 4 that the microstructure of the surface of the coating is highly ordered, and the protrusion pitch of the surface microstructure is 204.30um (X direction), 100um (Y direction), and the height is 41.82um (Z direction).
Fig. 5 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in the embodiment, and as can be seen from fig. 5, the contact angle reaches 92.51 degrees, and the ordered micro-nano structure antibacterial coating is a hydrophobic coating.
Example 3: the preparation method of the ordered multistage micro-nano structure antibacterial coating comprises the following steps:
weighing 60 parts of polybutadiene polyurethane, 15 parts of epoxy resin E51 and 5 parts of toluene according to the mass part ratio; adding polybutadiene polyurethane and epoxy resin E51 into a reaction vessel provided with a vacuum stirring system, uniformly mixing, adding toluene, and mixing for 3.5 hours to completely dissolve the polybutadiene polyurethane and the epoxy resin E51 until the mixture is clear and transparent, so as to obtain a solution A; wherein the polybutadiene polyurethane has a-NCO% content of 5%;
respectively weighing 30 parts of diethyl toluene diamine (DETDA) and 10 parts of toluene according to the mass part ratio; uniformly mixing diethyl toluenediamine (DETDA) and toluene to obtain a solution B;
thirdly, uniformly mixing the solution A and the solution B obtained in the second step according to the ratio of 1:1, filtering by a 200-mesh screen, standing for 30min at room temperature, and brushing on a sample plate;
fourthly, the sample plate in the third step is moved into an oven to be annealed for 2 hours at 50 ℃, and then is taken out after being crosslinked and cured for 24 hours at 80 ℃, thus obtaining the antibacterial coating with the highly ordered regular micro-nano structure on the surface.
Fig. 6 is a super-depth-of-field three-dimensional topography picture of the ordered micro-nano structure antibacterial coating prepared in the embodiment. It can be seen from fig. 7 that the microstructure of the surface of the coating is highly ordered, and the protrusion pitch of the surface microstructure is 248.50um (X direction), 246.80um (Y direction), and the height is 63.47um (Z direction).
Fig. 7 is a static water contact angle diagram of the ordered micro-nano structure antibacterial coating prepared in the embodiment, and as can be seen from fig. 7, the contact angle reaches 90.89 degrees, and the coating is a hydrophobic coating.
Claims (10)
1. A preparation method of an ordered multi-level micro-nano structure antibacterial coating is characterized by comprising the following steps:
firstly, respectively weighing 60-90 parts of polyurethane, 10-40 parts of epoxy resin and 5-10 parts of solvent according to the mass part ratio; adding polyurethane and epoxy resin into a reaction container provided with a vacuum stirring system, uniformly mixing, adding a solvent, and mixing for 2-4 hours to obtain a solution A; wherein the solvent is a medium polar solvent;
respectively weighing 20-30 parts of curing agent and 10-25 parts of solvent according to the mass part ratio; uniformly mixing a curing agent and a solvent to obtain a solution B; wherein the solvent is a medium polar solvent and is the same as the solvent in the step one;
thirdly, uniformly mixing the solution A and the solution B, filtering by using a screen, standing at room temperature, and brushing the mixture on the surface of the component to be protected;
fourthly, moving the component coated on the surface in the third step into an oven with the temperature of 50-60 ℃ for maintaining for 2-3 hours for annealing, raising the temperature to 80-90 ℃ for maintaining for 24-28 hours for crosslinking and curing, and obtaining the ordered multistage micro-nano structure antibacterial coating.
2. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1, wherein the polyurethane in the first step is polybutadiene polyurethane.
3. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 2, wherein the content of-NCO% in polybutadiene polyurethane is 4% -6%.
4. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the epoxy resin in the first step is bisphenol a type epoxy resin, and the type is E51 or E44.
5. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the solvent in the first step is toluene, benzene, xylene, ketones, esters, ethers or thiols.
6. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 5, characterized in that the ester solvent is ethyl acetate.
7. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the curing agent in the first step is di-o-chlorodiphenylamine methane or diethyl toluene diamine.
8. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the mixing ratio of the solution A and the solution B in the step three is (1.2-1.5): 1.
9. the preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the screen in the third step is 200-300 mesh.
10. The preparation method of the ordered multistage micro-nano structure antibacterial coating according to claim 1 or 2, characterized in that the brushing mode in the third step is brush coating, dip coating, roller coating or spray coating.
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| CN115975489A (en) * | 2023-01-06 | 2023-04-18 | 深圳陆城装饰设计工程有限公司 | Preparation method of ordered multi-stage micro-nano structure antibacterial coating |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327703A (en) * | 2014-10-15 | 2015-02-04 | 山东天汇防水材料有限公司 | Preparation method of composite superhydrophobic coating possessing abrasion-resistance performance |
| CN108250941A (en) * | 2018-01-22 | 2018-07-06 | 黑龙江省科学院高技术研究院 | A kind of low-surface-energy material with micro-nano groove structure and preparation method thereof |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104327703A (en) * | 2014-10-15 | 2015-02-04 | 山东天汇防水材料有限公司 | Preparation method of composite superhydrophobic coating possessing abrasion-resistance performance |
| CN108250941A (en) * | 2018-01-22 | 2018-07-06 | 黑龙江省科学院高技术研究院 | A kind of low-surface-energy material with micro-nano groove structure and preparation method thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115975489A (en) * | 2023-01-06 | 2023-04-18 | 深圳陆城装饰设计工程有限公司 | Preparation method of ordered multi-stage micro-nano structure antibacterial coating |
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