CN111073457A - Environment-friendly long-acting antibacterial coating and preparation method thereof - Google Patents
Environment-friendly long-acting antibacterial coating and preparation method thereof Download PDFInfo
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- CN111073457A CN111073457A CN201911407740.6A CN201911407740A CN111073457A CN 111073457 A CN111073457 A CN 111073457A CN 201911407740 A CN201911407740 A CN 201911407740A CN 111073457 A CN111073457 A CN 111073457A
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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
- C09D163/00—Coating compositions based on epoxy resins; Coating compositions based on derivatives of epoxy resins
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08G59/00—Polycondensates containing more than one epoxy group per molecule; Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups
- C08G59/18—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing
- C08G59/40—Macromolecules obtained by polymerising compounds containing more than one epoxy group per molecule using curing agents or catalysts which react with the epoxy groups ; e.g. general methods of curing characterised by the curing agents used
- C08G59/50—Amines
- C08G59/5046—Amines heterocyclic
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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
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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
- C09D5/14—Paints containing biocides, e.g. fungicides, insecticides or pesticides
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Abstract
The invention discloses an environment-friendly long-acting antibacterial coating and a preparation method thereof, belonging to the technical field of coatings. According to the invention, on one hand, a complex coacervation method is adopted to coat the cineole to microencapsulate the cineole, so that the compatibility of the cineole and the water-based epoxy resin is improved, meanwhile, the microencapsulation can also improve the thermal stability of the cineole and control the slow release of the cineole to achieve a more durable sterilization effect, and on the other hand, the monascus pigment is modified through the Mannich reaction of dimethylamine, acetaldehyde and the monascus pigment, so that the monascus pigment not only can be used as a curing agent to improve the chemical stability of the epoxy resin, but also can be used as a bactericide to synergistically play a sterilization role with the cineole, and the sterilization; in addition, the bactericide adopted in the formula of the coating is an extract of pure natural plants, and particularly, the cineole has the fragrance of cool herbal medicines, so that the prepared coating has excellent performances of safety, environmental protection, no toxicity, fragrant smell and the like.
Description
Technical Field
The invention belongs to the technical field of paint preparation, and particularly relates to an environment-friendly antibacterial paint and a preparation method thereof.
Background
The coating plays a great role in the building material field, can protect the main body material from being corroded, and can play a decorative effect. However, with the continuous development of coatings, people's demands on the coatings are not only just to protect substrates, but also environmental protection, safety, smell, antibacterial effect and the like of the coatings gradually become the consideration factors of consumers, and a small amount of antibacterial agent which has good adaptability and can exist stably is added into the coatings to prepare the antibacterial coatings, so that the coatings have effective antibacterial and antibacterial effects.
The monascus pigment is a traditional natural edible pigment in China, has the effect of inhibiting the activity of bacillus subtilis, staphylococcus aureus, escherichia coli and streptomyces griseus, and has excellent performances of excellent thermal stability, safety, no toxicity, no influence of iron ions and the like.
The cineole is the main component of aromatic essential oil secreted by eucalyptus leaf oil gland cells, has the fragrance of cool herbal medicine, has strong inhibition effect on escherichia coli and staphylococcus aureus, has the functions of mildew prevention, sterilization and corrosion prevention, and can be added into an air freshener for preventing and treating diseases such as respiratory tract infection, cold and the like to a certain extent.
Disclosure of Invention
In view of the above problems, the present invention aims to provide an antibacterial coating material with long-acting antibacterial effect, slow release, high stability, environmental protection and no harm, and a preparation method thereof.
The invention realizes the aim through the following technical scheme:
an environment-friendly long-acting antibacterial coating is composed of the following raw materials in parts by mass: 10-20 parts of microcapsule bactericide, 5-10 parts of modified monascus pigment, 60-80 parts of water-based epoxy resin and 50-80 parts of water;
the microcapsule bactericide is prepared by coating cineole by a complex coacervation method to make the cineole microencapsulated; the modified monascus pigment is prepared by performing Mannich reaction on acetaldehyde, dimethylamine and monascus pigment.
The preparation method of the microcapsule bactericide comprises the following steps:
(1) gelatin, Arabic gum and cineole are mixed according to the mass ratio of (4-5): (4-5): (4-8) dissolving in water, adding an emulsifier with the mass of 1.3-2.6 times that of the cineole, and homogenizing and emulsifying at high speed to form stable homogeneous emulsion;
(2) adjusting pH to 3.0-4.0 with 10% acetic acid solution, stirring at 50 deg.C for 2 hr, and cooling to 4 deg.C;
(3) adjusting the pH of the solution to 7.5-9.0 with 1% sodium hydroxide solution, adding a curing agent with the mass of 1.5-3.0 times of that of the cineole, and reacting for 3h at 50-70 ℃; washing with water or acetone, filtering, and freeze drying to obtain microcapsule bactericide.
The preparation method of the modified monascus pigment comprises the following steps:
(1) mixing the nonionic emulsifier and the deionized water according to the mass ratio of 1:3-1:4 to obtain a standby liquid;
(2) mixing monascus pigment, dimethylamine aqueous solution and deionized water according to the weight ratio of (1-3): (4-8): (4-6) mixing in a mass ratio, heating, adding an acetaldehyde solution with the mass of 1.5-2.0 times that of the monascus pigment, reacting for 1 hour, heating, and continuing to react for 2-3 hours;
(3) dehydrating in vacuum until no water is removed to obtain a material;
(4) adding a curing accelerator and a standby liquid into the material obtained in the step (3), wherein the mass ratio of the curing accelerator to the standby liquid is (1-2): (7-8): (4-6), and uniformly stirring to obtain the modified monascus pigment.
The rotating speed of the high-speed homogeneous emulsification in the step (1) is 10000-12000 r/min; the rotating speed of the low-speed stirring is 350-450 r/min.
The mass fraction of the dimethylamine aqueous solution in the step (2) is 40 percent; the mass fraction of the acetaldehyde solution is 40%.
And (3) heating to 70-85 ℃ in the step (2).
A preparation method of an environment-friendly antibacterial coating comprises the following steps:
(1) adding the microcapsule bactericide into a mixed solution of water and water-based epoxy resin, and stirring to obtain a mother solution of the environment-friendly bactericidal coating, wherein the mass ratio of the microcapsule bactericide to the water-based epoxy resin is (2-3): 4: 4.
(2) the modified monascus pigment and water are mixed according to the mass ratio (1-2): 4, uniformly mixing the mixture and the mother solution of the environment-friendly bactericidal coating according to the proportion of 1: and (3) mixing the components in the volume ratio to obtain the environment-friendly antibacterial coating.
According to the preparation method of the environment-friendly antibacterial coating, the emulsifier is one or two of span 80, span 20, tween 80, tween 60 and tween 65.
In the preparation method of the environment-friendly antibacterial coating, the curing agent is tannic acid or glutaraldehyde.
The preparation method of the environment-friendly antibacterial coating with the modified monascus pigment as the curing agent is characterized in that the non-ionic emulsifier is OP-4.
The preparation method of the environment-friendly antibacterial coating comprises the following step of preparing the waterborne resin into 828 waterborne epoxy resin, 862 waterborne epoxy resin, 3522-W-60A waterborne epoxy resin or 3540-WY-55A waterborne epoxy resin.
The invention has the beneficial effects that:
(1) the invention adopts a complex coacervation method to coat the cineole to lead the cineole to be microencapsulated, takes the Arabic gum and the gelatin as wall materials, coats the cineole to form a spherical structure, can improve the chemical stability of the cineole, can also improve the compatibility of the cineole and the water-based epoxy resin, and more importantly can control the cineole to be slowly released outwards so as to achieve the effect of long-acting sterilization and air purification.
(2) The Mannich reaction of acetaldehyde, dimethylamine and monascus pigment is adopted to modify the monascus pigment, so that the modified monascus pigment has the functions of curing and sterilizing, and the waterborne epoxy resin coating has excellent antibacterial property, safety and environmental protection, and can improve the properties of the waterborne epoxy resin, such as chemical stability and the like.
(3) In the coating, the modified monascus pigment has a sterilization effect and has a synergistic effect with eucalyptol, so that the antibacterial effect of the coating is more excellent.
(4) In the preparation process of the antibacterial coating, the formula of the water-based antibacterial coating takes eucalyptol and monascus pigment as raw materials, the eucalyptol and the monascus pigment belong to pure natural biomass, the environment-friendly coating belongs to green environment-friendly coatings, and the water-based antibacterial coating has the advantages of no toxicity, no harm, environmental friendliness, wide sources and the like.
Drawings
Fig. 1 is a scanned view of a eucalyptol microcapsule bactericide of the embodiment of the present invention, wherein a is the scanned view of the eucalyptol microcapsule bactericide with gum arabic as a wall material, and B is the scanned view of the eucalyptol microcapsule bactericide with gelatin as a wall material.
FIG. 2 is a Mannich reaction mechanism diagram of monascus pigment, acetaldehyde and dimethylamine.
Detailed Description
The present invention will be described in detail with reference to examples.
Example 1
Step 1: preparing the microcapsule bactericide:
(1) dissolving 2.0g gelatin, 2.0g acacia, 3.0g cineole in 60ml water to obtain solution, adding 3.9g emulsifier Tween-80, and homogenizing and emulsifying at high speed (12000r/min) for 5min to obtain stable homogeneous emulsion.
(2) Adjusting pH of the solution to 4.0 with 10% acetic acid solution, stirring at 50 deg.C at low speed (450r/min) for 2 hr, and cooling to 4 deg.C.
(3) Adjusting the pH of the solution to 8.0 by using 1% sodium hydroxide solution, adding 4.5g of glutaraldehyde with the mass fraction of 25%, reacting for 3h at 50 ℃, washing the microcapsule for 3 times by using water, filtering, and carrying out vacuum freeze drying for 24h to obtain the solid powder microcapsule bactericide.
Step 2: self-made modified monascus pigment:
(1) mixing a non-ionic emulsifier OP-4 and deionized water in a mass ratio of 1:3 to obtain a standby liquid;
(2) mixing and stirring 15g of monascus pigment, 60g of dimethylamine aqueous solution with the mass fraction of 40% and 60ml of deionized water, and heating to 50 ℃; adding 22.5g of 40 mass percent acetaldehyde solution into the mixture, reacting for 1 hour, and heating to 85 ℃ for reaction for 3 hours;
(3) the product is dehydrated in vacuum at 80 ℃, the vacuum degree is controlled at 700-;
(4) and (3) adding 10g of curing accelerator and 70g of standby liquid into 40g of dehydrated material, and uniformly stirring to obtain the self-made modified monascus pigment. .
And step 3: preparing an environment-friendly antibacterial coating:
(1) and (3) adding 20g of cineole microcapsule powder into a mixed solution of 40g of water and 40g of water-based epoxy resin, and magnetically stirring for 8min (350r/min) to obtain the mother solution of the environment-friendly bactericidal paint.
(2) Taking 15g of modified monacolin curing agent, uniformly mixing with 35g of water, and mixing with the mother liquor of the environment-friendly bactericidal coating according to the proportion of 1:3, and then carrying out performance test.
Example 2
Step 1: preparing the microcapsule bactericide:
(1) dissolving 2.0g gelatin, 2.0g acacia, 3.0g cineole in 60ml water to obtain solution, adding 3.9g emulsifier Tween-80, and homogenizing and emulsifying at high speed (12000r/min) for 5min to obtain stable homogeneous emulsion.
(2) Adjusting pH of the solution to 4.0 with 10% acetic acid solution, stirring at 50 deg.C at low speed (450r/min) for 2 hr, and cooling to 4 deg.C.
(3) Adjusting the pH of the solution to 8.0 by using 1% sodium hydroxide solution, adding 4.5g of glutaraldehyde with the mass fraction of 25%, reacting for 3h at 50 ℃, washing the microcapsule for 3 times by using water, filtering, and carrying out vacuum freeze drying for 24h to obtain the solid powder microcapsule bactericide.
Step 2: self-made modified monascus pigment:
(1) mixing a non-ionic emulsifier OP-4 and deionized water in a mass ratio of 1:3 to obtain a standby liquid;
(2) mixing and stirring 15g of monascus pigment, 60g of dimethylamine aqueous solution with the mass fraction of 40% and 60ml of deionized water, and heating to 50 ℃; adding 22.5g of 40 mass percent acetaldehyde solution into the mixture, reacting for 1 hour, and heating to 85 ℃ for reaction for 3 hours;
(3) the product is dehydrated in vacuum at 80 ℃, the vacuum degree is controlled at 700-;
(4) and (3) adding 10g of curing accelerator and 70g of standby liquid into 40g of dehydrated material, and uniformly stirring to obtain the self-made modified monascus pigment. .
And step 3: preparing an environment-friendly antibacterial coating:
(1) adding 30g of cineole microcapsule powder into a mixed solution of 40g of water and 40g of water-based epoxy resin, and magnetically stirring for 8min (350r/min) to obtain a mother solution of the environment-friendly bactericidal paint.
(2) Taking 15g of modified monacolin curing agent, uniformly mixing with 35g of water, and mixing with the mother liquor of the environment-friendly bactericidal coating according to the proportion of 1:3, and then carrying out performance test.
Example 3
Step 1: preparing the microcapsule bactericide:
(1) dissolving 2.0g gelatin, 2.0g acacia, 3.0g cineole in 60ml water to obtain solution, adding 3.9g emulsifier Tween-80, and homogenizing and emulsifying at high speed (12000r/min) for 5min to obtain stable homogeneous emulsion.
(2) Adjusting pH of the solution to 4.0 with 10% acetic acid solution, stirring at 50 deg.C at low speed (450r/min) for 2 hr, and cooling to 4 deg.C.
(3) Adjusting the pH of the solution to 8.0 by using 1% sodium hydroxide solution, adding 4.5g of glutaraldehyde with the mass fraction of 25%, reacting for 3h at 50 ℃, washing the microcapsule for 3 times by using water, filtering, and carrying out vacuum freeze drying for 24h to obtain the solid powder microcapsule bactericide.
Step 2: self-made modified monascus pigment:
(1) mixing a non-ionic emulsifier OP-4 and deionized water in a mass ratio of 1:3 to obtain a standby liquid;
(2) mixing and stirring 15g of monascus pigment, 60g of dimethylamine aqueous solution with the mass fraction of 40% and 60ml of deionized water, and heating to 50 ℃; adding 22.5g of 40 mass percent acetaldehyde solution into the mixture, reacting for 1 hour, and heating to 85 ℃ for reaction for 3 hours;
(3) the product is dehydrated in vacuum at 80 ℃, the vacuum degree is controlled at 700-;
(4) and (3) adding 10g of curing accelerator and 70g of standby liquid into 40g of dehydrated material, and uniformly stirring to obtain the self-made modified monascus pigment. .
And step 3: preparing an environment-friendly antibacterial coating:
(1) adding 30g of cineole microcapsule powder into a mixed solution of 40g of water and 40g of water-based epoxy resin, and magnetically stirring for 8min (350r/min) to obtain a mother solution of the environment-friendly bactericidal paint.
(2) Taking 15g of modified monacolin curing agent, uniformly mixing with 35g of water, and mixing with the mother liquor of the environment-friendly bactericidal coating according to the proportion of 1:4, and then carrying out performance test.
The specific technical indexes are shown in table 1:
as can be seen from Table 1: the antibacterial performance of the coating is increased with the increase of the modified monascus pigment curing agent, the curing time is shortened, the bactericidal performance of the coating is greatly improved with the increase of the addition amount of the eucalyptol microcapsule, but from the comprehensive performance, the comprehensive effect example 2(11:30) > example 3(11:40) > example 1(1:2) of the three proportions of the modified monascus pigment and the microcapsule bactericide is that the mass ratio is 11:30, the coating has wide, efficient and lasting bactericidal and inhibiting capabilities on staphylococcus aureus and escherichia coli, the curing time of the coating is shortened, and the construction inconvenience is reduced.
Comparative example 1 (Monascus non-modified)
In comparative example 1, the raw materials and process for preparing the coating are the same as those in example 3 except that the monacolin is not modified, and the method specifically comprises the following steps:
step 1: preparing the microcapsule bactericide:
(1) dissolving 2.0g gelatin, 2.0g acacia, 3.0g cineole in 60ml water to obtain solution, adding 3.9g emulsifier Tween-80, and homogenizing and emulsifying at high speed (12000r/min) for 5min to obtain stable homogeneous emulsion.
(2) Adjusting pH of the solution to 4.0 with 10% acetic acid solution, stirring at 50 deg.C at low speed (450r/min) for 2 hr, and cooling to 4 deg.C.
(3) Adjusting the pH of the solution to 8.0 by using 1% sodium hydroxide solution, adding 4.5g of glutaraldehyde with the mass fraction of 25%, reacting for 3h at 50 ℃, washing the microcapsule for 3 times by using water, filtering, and carrying out vacuum freeze drying for 24h to obtain the solid powder microcapsule bactericide.
And step 3: preparing an environment-friendly antibacterial coating:
(1) adding 30g of cineole microcapsule powder into a mixed solution of 40g of water and 40g of water-based epoxy resin, and magnetically stirring for 8min (350r/min) to obtain a mother solution of the environment-friendly bactericidal paint.
(2) Taking 15g of monacolin and 35g of water, uniformly mixing, and mixing with the mother solution of the environment-friendly bactericidal coating according to the proportion of 1:4, and then carrying out performance test.
The specific technical indexes are shown in Table 2
| Item | Example 3 | Comparative example 1 | Test standard |
| Time to surface dry (min) | 19 | 27 | GB/T1728-79 |
| Actual drying time (h) | 21 | 24 | GB/T1729-79 |
| Adhesion (grade) | 1 | 1 | GB/T1720-79 |
| Staphylococcus aureus antibacterial ratio (%) | 95.23％ | 94.36％ | GB/T21866-2008 |
| Antibacterial ratio of Escherichia coli (%) | 96.55％ | 93.98％ | GB/T21866-2008 |
Comparing the coating prepared in comparative example 1 with the coating prepared in example 3, it was found that: the modified monascus pigment can be used as a curing agent, so that the curing time of the coating is greatly shortened, and can also be used as an antibacterial agent, so that the antibacterial performance of the coating is improved.
Claims (10)
1. The environment-friendly long-acting antibacterial coating is characterized by comprising the following raw materials in parts by mass: 10-20 parts of microcapsule bactericide, 5-10 parts of modified monascus pigment, 60-80 parts of water-based epoxy resin and 50-80 parts of water;
the microcapsule bactericide is prepared by coating cineole by a complex coacervation method to make the cineole microencapsulated; the modified monascus pigment is prepared by performing Mannich reaction on acetaldehyde, dimethylamine and monascus pigment.
2. The environment-friendly long-acting antibacterial coating according to claim 1, wherein the mass ratio of the microcapsule bactericide to the modified monascus pigment is 11: 30.
3. The environmentally friendly long-acting antibacterial coating according to claim 1, wherein the preparation method of the microcapsule bactericide comprises the following steps:
(1) gelatin, Arabic gum and cineole are mixed according to the mass ratio of (4-5): (4-5): (4-8) dissolving in water, adding an emulsifier with the mass of 1.3-2.6 times that of the cineole, and homogenizing and emulsifying at high speed to form stable homogeneous emulsion;
(2) adjusting pH to 3.0-4.0 with 10% acetic acid solution, stirring at 50 deg.C for 2 hr, and cooling to 4 deg.C;
(3) adjusting the pH of the solution to 7.5-9.0 with 1% sodium hydroxide solution, adding a curing agent with the mass of 1.5-3.0 times of that of the cineole, and reacting for 3h at 50-70 ℃; washing with water or acetone, filtering, and freeze drying to obtain microcapsule bactericide.
4. The environment-friendly long-acting antibacterial coating according to claim 1, wherein the preparation method of the modified monascus pigment comprises the following steps:
(1) mixing the nonionic emulsifier and the deionized water according to the mass ratio of 1:3-1:4 to obtain a standby liquid;
(2) mixing monascus pigment, dimethylamine aqueous solution and deionized water according to the weight ratio of (1-3): (4-8): (4-6) mixing in a mass ratio, heating, adding an acetaldehyde solution with the mass of 1.5-2.0 times that of the monascus pigment, reacting for 1 hour, heating, and continuing to react for 2-3 hours;
(3) dehydrating in vacuum until no water is removed to obtain a material;
(4) adding a curing accelerator and a standby liquid into the material obtained in the step (3), wherein the mass ratio of the curing accelerator to the standby liquid is (1-2): (7-8): (4-6), and uniformly stirring to obtain the modified monascus pigment.
5. The environmentally friendly long-acting antibacterial coating as claimed in claim 3, wherein the rotation speed of the high-speed homogeneous emulsification in (1) is 10000-12000 r/min; the rotating speed of the low-speed stirring is 350-450 r/min.
6. The environment-friendly long-acting antibacterial coating according to claim 4, wherein the mass fraction of the dimethylamine aqueous solution in the step (2) is 40%; the mass fraction of the acetaldehyde solution is 40%.
7. The environmentally friendly long-acting antibacterial coating according to claim 4, wherein the temperature in the step (2) is raised to 70-85 ℃.
8. The environmentally friendly long-acting antibacterial coating according to claim 4, wherein the non-ionic emulsifier is OP-4.
9. The preparation method of the environment-friendly antibacterial coating is characterized by comprising the following steps:
(1) adding the microcapsule bactericide into a mixed solution of water and water-based epoxy resin, and stirring to obtain a mother solution of the environment-friendly bactericidal coating, wherein the mass ratio of the microcapsule bactericide to the water-based epoxy resin is (2-3): 4: 4;
(2) the modified monascus pigment and water are mixed according to the mass ratio (1-2): 4, uniformly mixing the mixture and the mother solution of the environment-friendly bactericidal coating according to the proportion of 1: and (3) mixing the components in the volume ratio to obtain the environment-friendly antibacterial coating.
10. The method for preparing the environment-friendly antibacterial coating according to claim 9, wherein the emulsifier is one or two of span 80, span 20, tween 80, tween 60 and tween 65;
the curing agent is tannic acid or glutaraldehyde;
the waterborne resin is 828 waterborne epoxy resin, 862 waterborne epoxy resin, 3522-W-60A waterborne epoxy resin or 3540-WY-55A waterborne epoxy resin.
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| CN116082874A (en) * | 2023-01-04 | 2023-05-09 | 浙江丰虹新材料股份有限公司 | Efficient durable mildew-proof coating and preparation method thereof |
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Application publication date: 20200428 |