CN112778451A - Antibacterial and antiviral acrylic emulsion and preparation method thereof - Google Patents
Antibacterial and antiviral acrylic emulsion and preparation method thereof Download PDFInfo
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Abstract
The invention discloses an antibacterial and antiviral acrylic emulsion and a preparation method thereof. The antibacterial and antiviral acrylic emulsion uses anionic and nonionic emulsifiers with excellent water resistance, and the prepared emulsion has excellent performance through reasonable monomer proportion and functional monomer selection. Meanwhile, the prepared acrylic emulsion has continuous and effective antibacterial and antiviral effects by adding the rare earth micro powder and the silver ion solution, and the high-grade emulsion paint prepared from the acrylic emulsion has excellent water resistance, wet scrubbing property and stain resistance, and long-lasting antibacterial and antiviral effects, and is safe and effective.
Description
Technical Field
The invention relates to the technical field of acrylic emulsion and preparation thereof, in particular to antibacterial and antiviral acrylic emulsion and a preparation method thereof.
Background
With increasing attention of consumers to environmental protection and health problems, functional latex paints such as alkylphenol polyoxyethylene ether compounds (APEO), formaldehyde-free formaldehyde-removing latex paints with extremely low odor, zero-additive latex paints, anti-graffiti latex paints and the like have gradually increased in proportion in the whole building coating. In recent years, paints having antibacterial and antiviral effects have been on the market, but the quality of the products thereof is not uniform. Recently, the standards of the T/CNCIA 01014-. The current coatings with antibacterial and antiviral effects on the market mainly comprise the following types:
1. the antibacterial and antiviral effects are achieved by adding metal ion solutions such as silver ion solution, copper ion solution, zinc ion solution, etc. Of these, silver ion solutions are the most effective, followed by copper ion solutions, but copper ion solutions require very high addition levels to achieve good results, and have a number of disadvantages in coating applications, such as affecting the appearance and storage stability of the coating.
2. By adding nano metal or metal oxide such as nano silver, nano copper, nano zinc and the like, the antibacterial and antiviral effects of the nano metal material particles are not as ideal as those of a solution state. If the "filler" is used by increasing the amount of addition, problems such as excessive cost and poor storage stability are caused.
3. Bacteria and viruses are killed by a photocatalyst technology represented by nano titanium dioxide, but the practicability of the photocatalyst technology is not really accepted by the market.
It is seen that improvements and enhancements to the prior art are needed.
Disclosure of Invention
In view of the defects of the prior art, the invention aims to provide an antibacterial and antiviral acrylic emulsion and a preparation method thereof, and aims to solve the technical problems of poor antibacterial and antiviral effects, poor storage stability and high cost of the coating in the prior art.
In order to achieve the purpose, the invention adopts the following technical scheme:
an antibacterial antiviral acrylic emulsion comprises the following raw materials in parts by weight: 90-110 parts of deionized water, 0.02-0.15 part of rare earth micro powder, 0.5-2 parts of silver ion solution, 1-8 parts of emulsifier, 0.2-3 parts of initiator, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide.
In the antibacterial and antiviral acrylic emulsion, the rare earth micro powder is one or two of boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth. .
In the antibacterial and antiviral acrylic emulsion, the rare earth micro powder is crystal micro powder with the particle size not more than 120 nanometers.
In the antibacterial and antiviral acrylic emulsion, the silver ion solution is a silver-based antibacterial agent.
In the antibacterial and antiviral acrylic emulsion, the emulsifier is composed of an anionic emulsifier and a nonionic emulsifier.
In the antibacterial and antiviral acrylic emulsion, the anionic emulsifier is one or two of alkyl sodium sulfate and alkyl sodium sulfonate.
In the antibacterial and antiviral acrylic emulsion, the nonionic emulsifier is alkyl alcohol polyoxyethylene ether containing 9-11 EO.
In the antibacterial and antiviral acrylic emulsion, the initiator is one or more than two of ammonium persulfate, potassium persulfate and sodium persulfate.
A preparation method of antibacterial and antiviral acrylic emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 40-50 parts of deionized water, 0-5 parts of emulsifier and all rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, stirring, heating to make the temperature in the reaction kettle reach 60-90 ℃, keeping the temperature and continuously stirring to prepare a bottom feed liquid A for later use;
s002, preparing a pre-emulsion B: adding 40-50 parts of deionized water, 1-8 parts of emulsifier, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to obtain a uniform pre-emulsion B, and stirring for later use;
s003, preparing an initiator solution C: adding the rest deionized water and 0.2-3 parts of initiator into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the deionized water and the initiator are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 60-90 ℃, adding 4-10% of the total amount of the pre-emulsion B and 20-50% of the total amount of the initiator solution C into the bottom liquid A in the kettle, reacting for 5-30 minutes, dropwise adding the rest of the pre-emulsion B and the initiator solution C into the reaction kettle simultaneously through a constant flow pump feeding device and a constant flow dropwise adding metering device, controlling the dropwise adding time to be 150 plus materials for 240 minutes, and finishing dropwise adding the initiator solution C0-30 minutes later than the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 60-90 ℃, preserving the heat for 1-2 hours, then cooling, adjusting the pH of the emulsion to be 7.0-9.0 by using an ammonia water solution, stirring for 0.5 hour, then adding all silver ion solutions, stirring for 0.5 hour, filtering and discharging to obtain the antibacterial and antiviral acrylic emulsion.
Has the advantages that:
the invention provides an antibacterial and antiviral acrylic emulsion and a preparation method thereof, wherein the antibacterial and antiviral acrylic emulsion uses anionic and nonionic emulsifiers with excellent water resistance, and the prepared emulsion has the characteristics of excellent water resistance, excellent wet scrubbing property and excellent stain resistance through reasonable monomer proportion and functional monomer selection, and can meet the requirements of high-grade emulsion paints. Meanwhile, the prepared acrylic emulsion has continuous and effective antibacterial and antiviral effects by adding the rare earth micro powder and the silver ion solution, and the high-grade latex paint prepared from the acrylic emulsion has excellent antibacterial and antiviral properties.
Detailed Description
The invention provides an antibacterial and antiviral acrylic emulsion and a preparation method thereof, and in order to make the purposes, technical schemes and effects of the invention clearer and clearer, the invention is further described in detail with reference to the following examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
An antibacterial antiviral acrylic emulsion comprises the following raw materials in parts by weight: 90-110 parts of deionized water, 0.02-0.15 part of rare earth micro powder, 0.5-2 parts of silver ion solution, 1-8 parts of emulsifier, 0.2-3 parts of initiator, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide.
The rare earth micro powder and the silver ion solution provide antibacterial and antiviral effects; the emulsifier provides emulsification, dispersion and stabilization; the initiator is a water-soluble thermal initiator, and can provide a proper polymerization rate and reduce the gel amount; isooctyl acrylate and butyl acrylate can provide good flexibility for the chain segment of the latex particle by being taken as soft monomers; methyl methacrylate as a hard monomer can provide good rigidity for the chain segment of the latex particle; acrylic acid, methacrylic acid, acrylamide and methacrylamide which are taken as functional monomers can not only improve the mechanical stability, calcium ion stability, freeze-thaw stability and storage stability of the emulsion, but also improve the wet scrubbing property, the stain resistance and the like of the emulsion.
The rare earth micro powder is one or two of boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth. The lanthanide rare earth includes 17 elements of lanthanide elements in the periodic table of chemical elements and closely related elements of scandium and yttrium. The rare earth micro powder is in a metastable state of an electron layer, can absorb energy (light energy, heat energy and energy in other forms) to generate electrons to jump to a higher layer, and can release energy when the electrons of the higher layer are restored to the original electron layer. Wherein the boron molybdate crystal of lanthanide rare earth and the iron oxide crystal of lanthanide rare earth can release terahertz energy. Terahertz energy has a variety of beneficial effects, one of which is that it can resist bacteria and viruses.
The rare earth boron molybdate crystal can release energy with the wavelength of about 1.5T, the rare earth iron oxide crystal can release energy with the wavelength of about 0.5T, and the mixture of the rare earth boron molybdate crystal and the rare earth iron oxide crystal can release energy with the wavelength of 0.5T-1.5T, namely terahertz energy (THz energy). The terahertz energy belongs to far infrared wavelength energy, is harmless to the environment and human beings, and can also play a health care role to the human bodies. The absorption and release of the energy of the rare earth micro powder are synchronously and continuously carried out, attenuation does not exist, and the antibacterial and antiviral effects can be continuously ensured.
Further, the rare earth micro powder is crystal micro powder with the particle size not more than 120 nanometers. The smaller crystal grain size can improve the flexibility of the acrylic emulsion and is more beneficial to the homogeneous distribution of the rare earth micro powder in a system.
The silver ion solution is a silver-based antibacterial agent. The antibacterial and antiviral effects can be further improved by adding silver-based antibacterial agent. Silver in the silver ion solution exists in an ion form, the activity is high, the silver ion solution still exists in the silver ion form after killing bacteria, mould and virus, the attenuation is hardly caused, and the effective time is long. The silver antibacterial agent can be one or more of silver antibacterial agent DM series products DM-Ag01, DM-Ag02, DM-Ag06, DM-Ag08, DM-830, DM-831, DM-832, DM-530, DM-531 and DM-532 of New materials Co., Ltd, Guangdong Dy.
The emulsifier is composed of an anionic emulsifier and a nonionic emulsifier. The anionic emulsifier and the nonionic emulsifier are used together to improve the emulsifying effect.
Further, the anionic emulsifier is one or two of sodium alkyl sulfate and sodium alkyl sulfonate.
Further, the nonionic emulsifier is alkyl alcohol polyoxyethylene ether containing 9-11 EO.
The initiator is one or more than two of ammonium persulfate, potassium persulfate and sodium persulfate. The ammonium persulfate, the potassium persulfate and the sodium persulfate are cheap, so that the production cost can be reduced.
The preparation method of the antibacterial and antiviral acrylic emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 40-50 parts of deionized water, 0-5 parts of emulsifier and all rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, stirring, heating to make the temperature in the reaction kettle reach 60-90 ℃, keeping the temperature and continuously stirring to prepare a bottom feed liquid A for later use;
s002, preparing a pre-emulsion B: adding 40-50 parts of deionized water, 1-8 parts of emulsifier, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to obtain a uniform pre-emulsion B, and stirring for later use;
s003, preparing an initiator solution C: adding the rest deionized water and 0.2-3 parts of initiator into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the deionized water and the initiator are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 60-90 ℃, adding 4-10% of the total amount of the pre-emulsion B and 20-50% of the total amount of the initiator solution C into the bottom liquid A in the reaction kettle, reacting for 5-30 minutes, dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle at the same time through a constant flow pump feeding device and a constant flow dropwise adding metering device, controlling the dropwise adding time to be 150-240 minutes, and finishing dropwise adding the initiator solution C0-30 minutes later than the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 60-90 ℃, preserving the heat for 1-2 hours, then cooling, adjusting the pH of the emulsion to be 7.0-9.0 by using an ammonia water solution, stirring for 0.5 hour, then adding all the silver ion solution, stirring for 0.5 hour, filtering and discharging to obtain the antibacterial and antiviral acrylic emulsion.
The antibacterial and antiviral acrylic emulsion is used for preparing high-grade interior wall latex paint, and the performance of the obtained high-grade interior wall latex paint is tested according to GB/T9780-.
Example 1
The antibacterial and antiviral acrylic emulsion comprises the following components in parts by weight: 95 parts of deionized water, 2 parts of emulsifier, 0.04 part of rare earth micro powder, 0.5 part of silver ion solution, 0.4 part of initiator, 5 parts of isooctyl acrylate, 55 parts of butyl acrylate, 35 parts of methyl methacrylate, 0.4 part of acrylic acid, 0.4 part of methacrylic acid, 0.4 part of acrylamide and 0.4 part of methacrylamide.
The rare earth micro powder is prepared by mixing boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth in a ratio of 1: 0.6.
The silver ion solution is DM-830 of a silver antibacterial agent DM series product of Guangdong Dimei new material company Limited.
The emulsifier is a composite emulsifier formed by mixing an anionic emulsifier and a nonionic emulsifier, the anionic emulsifier adopts sodium alkyl sulfate, and the nonionic emulsifier adopts alkyl alcohol polyoxyethylene ether containing 9 EO.
Ammonium persulfate is adopted as the initiator.
The preparation method of the emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 40 parts of deionized water, 1 part of emulsifier and 0.04 part of rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, and heating until the temperature in the kettle reaches 76 ℃;
s002, preparing a pre-emulsion B: adding all isooctyl acrylate, butyl acrylate, methyl methacrylate, acrylic acid, methacrylic acid, acrylamide, methacrylamide, 1 part of emulsifier and 30 parts of deionized water into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to form uniform pre-emulsion, and stirring for 10 minutes for later use;
s003, preparing an initiator solution C: adding 0.4 part of initiator and the rest deionized water into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the rest deionized water are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 76 ℃, adding 5% of the total amount of the pre-emulsion B and 20% of the total amount of the initiator solution C into the reaction kettle, after 5 minutes, simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle by using a constant flow pump feeding device and a constant current dropwise adding metering device, controlling the dropwise adding time to be 180 minutes, and finishing dropwise adding the initiator solution C5 minutes later than the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 76-78 ℃, preserving the heat for 1.5 hours, reducing the temperature, adjusting the pH value to 7.5 by using ammonia water, stirring for 0.5 hour, adding all silver ion solution, stirring for 0.5 hour, filtering and discharging to obtain the acrylic emulsion with the antibacterial and antiviral effects.
The emulsion obtained has a solid content of 48.8%, a viscosity of 300cps, a pH of 7.6, and a particle size of 110 nm.
The emulsion is used for preparing high-grade interior wall latex paint, and the addition amount of the emulsion is 35%. The prepared latex paint has no obvious change after being stored for 30 days, the water resistance of a paint film is not abnormal within 96 hours, the wet scourability exceeds 10000 times, and the stain resistance durability respectively reach 75.5 percent and 62.0 percent. The antibacterial performance and the antibacterial durability respectively reach more than 99.99 percent and 99.80 percent, the antifungal performance and the antifungal durability respectively reach 0 grade and 0 grade, the antiviral performance and the antiviral durability H3N2 respectively reach more than 99.99 percent and 99.52 percent, and the antiviral performance and the antiviral durability EV71 respectively reach more than 99.99 percent and 93.35 percent.
Example 2:
the antibacterial and antiviral acrylic emulsion comprises the following components in parts by weight: 100 parts of deionized water, 3 parts of emulsifier, 0.1 part of rare earth micro powder, 1 part of silver ion solution, 1 part of initiator, 10 parts of isooctyl acrylate, 50 parts of butyl acrylate, 40 parts of methyl methacrylate, 1 part of acrylic acid, 1 part of methacrylic acid, 1 part of acrylamide and 1 part of methacrylamide.
Wherein the rare earth micro powder is prepared by mixing boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth in a ratio of 1: 0.8.
The silver ion solution adopts DM-Ag01 of silver antibacterial agent DM series products of Guangdong Dimei new material company, Inc.
The emulsifier is a composite emulsifier formed by mixing an anionic emulsifier and a nonionic emulsifier, the anionic emulsifier adopts sodium alkyl sulfate, and the nonionic emulsifier adopts alkyl alcohol polyoxyethylene ether containing 10 EO.
The initiator is sodium persulfate.
The preparation method of the emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 45 parts of deionized water, 2 parts of emulsifier and 0.1 part of rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, and heating until the temperature in the kettle reaches 80 ℃;
s002, preparing a pre-emulsion B: adding all isooctyl acrylate, butyl acrylate, methyl methacrylate, acrylic acid, methacrylic acid, acrylamide, methacrylamide, 1 part of emulsifier and 35 parts of deionized water into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to form uniform pre-emulsion, and stirring for 10 minutes for later use;
s003, preparing an initiator solution C: adding 1 part of initiator and the rest deionized water into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the rest deionized water are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 80 ℃, adding 9% of the total amount of the pre-emulsion B and 22% of the total amount of the initiator solution C into the reaction kettle, after 8 minutes, simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle by using a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding time is controlled to be 210 minutes, and the dropwise adding of the initiator solution C is finished 15 minutes later than that of the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 80-82 ℃, preserving the heat for 1.5 hours, reducing the temperature, adjusting the pH to 7.0 by using ammonia water, stirring for 0.5 hour, adding all the silver ion solution, stirring for 0.5 hour, filtering and discharging to obtain the acrylic emulsion with the antibacterial and antiviral effects.
The emulsion obtained had a solid content of 49.6%, a viscosity of 350cps, a pH of 7.2 and a particle size of 125 nm.
The emulsion is used for preparing high-grade interior wall latex paint, and the addition amount of the emulsion is 35%. The prepared latex paint has no obvious change after being stored for 30 days, the water resistance of a paint film is not abnormal within 96 hours, the wet scourability exceeds 10000 times, and the stain resistance durability respectively reach 77.0 percent and 64.0 percent. The antibacterial performance and the antibacterial durability respectively reach more than 99.99 percent and 99.90 percent, the antifungal performance and the antifungal durability respectively reach 0 grade and 0 grade, the antiviral performance and the antiviral durability H3N2 respectively reach more than 99.99 percent and 99.80 percent, and the antiviral performance and the antiviral durability EV71 respectively reach more than 99.99 percent and 93.85 percent.
Example 3:
the antibacterial and antiviral acrylic emulsion comprises the following components in parts by weight: 110 parts of deionized water, 5 parts of emulsifier, 0.12 part of rare earth micro powder, 1.5 parts of silver ion solution, 1.5 parts of initiator, 15 parts of isooctyl acrylate, 45 parts of butyl acrylate, 45 parts of methyl methacrylate, 1.5 parts of acrylic acid, 1.5 parts of methacrylic acid, 1.5 parts of acrylamide and 1.5 parts of methacrylamide.
Wherein the rare earth micro powder is prepared by mixing boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth in a ratio of 0.6: 1.
The silver ion solution is DM-Ag02 of New Material Co., Ltd.
The emulsifier is a composite emulsifier formed by mixing an anionic emulsifier and a nonionic emulsifier. Still further, wherein the anionic emulsifier employs sodium alkyl sulfonate; the nonionic emulsifier adopts alkyl alcohol polyoxyethylene ether with 11 EO.
The initiator is potassium persulfate.
The preparation method of the emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 50 parts of deionized water, 3 parts of emulsifier and 0.12 part of rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, and heating until the temperature in the kettle reaches 82 ℃;
s002, preparing a pre-emulsion B: adding all isooctyl acrylate, butyl acrylate, methyl methacrylate, acrylic acid, methacrylic acid, acrylamide, methacrylamide, 2 parts of emulsifier and 35 parts of deionized water into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to form uniform pre-emulsion, and stirring for 10 minutes for later use;
s003, preparing an initiator solution C: adding 1.5 parts of initiator and the rest deionized water into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the rest deionized water are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 82 ℃, adding 8% of the total amount of the pre-emulsion B and 25% of the total amount of the initiator solution C into the reaction kettle, after 20 minutes, simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle by using a constant flow pump feeding device and a constant current dropwise adding metering device, controlling the dropwise adding time to be 180 minutes, and finishing dropwise adding the initiator solution C10 minutes later than the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 82-84 ℃, preserving the heat for 1 hour, reducing the temperature, adjusting the pH to be 7.6 by using ammonia water, stirring for 0.5 hour, adding all silver ion solution, filtering and discharging to obtain the acrylic emulsion with the antibacterial and antiviral effects.
The emulsion had a solids content of 49.8%, a viscosity of 2800cps, a pH of 7.6, and a particle size of 100 nm.
The emulsion is used for preparing high-grade interior wall latex paint, and the addition amount of the emulsion is 35%. The prepared latex paint has no obvious change after being stored for 30 days, the water resistance of a paint film is not abnormal within 96 hours, the wet scourability exceeds 10000 times, and the stain resistance durability respectively reach 76.0 percent and 63.0 percent. The antibacterial performance and the antibacterial durability respectively reach more than 99.99 percent and more than 99.99 percent, the antifungal performance and the antifungal durability respectively reach 0 grade and 0 grade, the antiviral performance and the antiviral durability H3N2 respectively reach more than 99.99 percent and 99.96 percent, and the antiviral performance and the antiviral durability EV71 respectively reach more than 99.99 percent and 95.66 percent.
Example 4:
the antibacterial and antiviral acrylic emulsion comprises the following components in parts by weight: 90 parts of deionized water, 1 part of emulsifier, 0.02 part of rare earth micro powder, 1.88 parts of silver ion solution, 0.2 part of initiator, 20 parts of isooctyl acrylate, 45 parts of methyl methacrylate, 2.5 parts of acrylic acid, 2 parts of methacrylic acid, 2.5 parts of acrylamide and 2 parts of methacrylamide.
The rare earth micro powder is prepared by mixing boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth in a ratio of 1:0.
The silver ion solution is DM-Ag06 of New Material Co., Ltd.
The emulsifier is a composite emulsifier formed by mixing an anionic emulsifier and a nonionic emulsifier. Still further, wherein the anionic emulsifier employs sodium alkyl sulfonate; the nonionic emulsifier adopts alkyl alcohol polyoxyethylene ether with 10 EO.
The initiator is potassium persulfate.
The preparation method of the emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 50 parts of deionized water, 0.6 part of emulsifier and 0.02 part of rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, and heating until the temperature in the kettle reaches 84 ℃;
s002, preparing a pre-emulsion B: adding all isooctyl acrylate, methyl methacrylate, acrylic acid, methacrylic acid, acrylamide, methacrylamide, 0.4 part of emulsifier and 30 parts of deionized water into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to form uniform pre-emulsion, and stirring for 10 minutes for later use;
s003, preparing an initiator solution C: adding 0.2 part of initiator and the rest deionized water into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the rest deionized water are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 84 ℃, adding 8% of the total amount of the pre-emulsion B and 20% of the total amount of the initiator solution C into the reaction kettle, after 20 minutes, simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle by using a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding time is controlled to be 200 minutes, and the dropwise adding of the initiator solution C is finished 10 minutes later than that of the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 82-84 ℃, preserving the heat for 1 hour, reducing the temperature, adjusting the pH to be 7.6 by using ammonia water, stirring for 0.5 hour, adding all silver ion solution, filtering and discharging to obtain the acrylic emulsion with the antibacterial and antiviral effects.
The emulsion obtained has a solid content of 45.1%, a viscosity of 600cps, a pH of 7.4, and a particle size of 110 nm.
The obtained emulsion is used for preparing high-grade interior wall latex paint, and the addition amount of the emulsion is 38%. The prepared latex paint has no obvious change after being stored for 30 days, the water resistance of a paint film is not abnormal within 96 hours, the wet scourability exceeds 10000 times, and the stain resistance durability respectively reach 75.5 percent and 62.0 percent. The antibacterial performance and the antibacterial durability respectively reach 99.99 percent and 96.79 percent, the antifungal performance and the antifungal durability respectively reach 0 grade and 0 grade, the antiviral performance and the antiviral durability H3N2 respectively reach 99.99 percent and 99.22 percent, and the antiviral performance and the antiviral durability EV71 respectively reach 96.89 percent and 92.67 percent.
Example 5:
the antibacterial and antiviral acrylic emulsion comprises the following components in parts by weight: 110 parts of deionized water, 8 parts of emulsifier, 0.15 part of rare earth micro powder, 2 parts of silver ion solution, 3 parts of initiator, 60 parts of butyl acrylate, 0.2 part of acrylic acid, 10 parts of methacrylic acid and 0.2 part of acrylamide.
Wherein the rare earth micro powder is prepared by mixing boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth in a ratio of 0: 1.
The silver ion solution is DM-Ag08 of New Material Co., Ltd.
The emulsifier is a composite emulsifier formed by mixing an anionic emulsifier and a nonionic emulsifier. Still further, wherein the anionic emulsifier employs sodium alkyl sulfonate; the nonionic emulsifier adopts alkyl alcohol polyoxyethylene ether with 11 EO.
The initiator is ammonium persulfate.
The preparation method of the emulsion comprises the following steps:
s001, preparing a base material liquid A: adding 60 parts of deionized water, 5 parts of emulsifier and 0.15 part of rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, and heating until the temperature in the kettle reaches 84 ℃;
s002, preparing a pre-emulsion B: adding all butyl acrylate, acrylic acid, methacrylic acid and acrylamide, 3 parts of emulsifier and 30 parts of deionized water into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to obtain uniform pre-emulsion, and stirring for 10 minutes for later use;
s003, preparing an initiator solution C: adding 3 parts of initiator and the rest deionized water into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the initiator and the rest deionized water are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 86 ℃, adding 10% of the total amount of the pre-emulsion B and 25% of the total amount of the initiator solution C into the reaction kettle, after 20 minutes, simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle by using a constant flow pump feeding device and a constant current dropwise adding metering device, wherein the dropwise adding time is controlled to be 190 minutes, and the dropwise adding of the initiator solution C is finished 10 minutes later than that of the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 84-86 ℃, preserving the heat for 1 hour, reducing the temperature, adjusting the pH to 7.6 by using ammonia water, stirring for 0.5 hour, adding all silver ion solution, filtering and discharging to obtain the acrylic emulsion with the antibacterial and antiviral effects.
The emulsion obtained had a solids content of 39.4%, a viscosity of 300cps, a pH of 7.6, and a particle size of 115 nm.
The obtained emulsion is used for preparing high-grade interior wall latex paint, and the addition amount of the emulsion is 40%. The prepared latex paint has no obvious change after being stored for 30 days, the water resistance of a paint film is not abnormal within 96 hours, the wet scourability exceeds 10000 times, and the stain resistance durability respectively reach 77.2 percent and 62.8 percent. The antibacterial performance and the antibacterial durability respectively reach 99.99 percent and 99.99 percent, the antifungal performance and the antifungal durability respectively reach 0 grade and 0 grade, the antiviral performance and the antiviral durability H3N2 respectively reach 99.99 percent and 99.82 percent, and the antiviral performance and the antiviral durability EV71 respectively reach 99.99 percent and 96.77 percent.
The latex paint performance parameters set forth in examples 1-5 above are shown in the following table:
it should be understood that equivalents and modifications of the technical solution and inventive concept thereof may occur to those skilled in the art, and all such modifications and alterations should fall within the scope of the appended claims.
Claims (9)
1. The antibacterial and antiviral acrylic emulsion is characterized by comprising the following raw materials in parts by weight: 90-110 parts of deionized water, 0.02-0.15 part of rare earth micro powder, 0.5-2 parts of silver ion solution, 1-8 parts of emulsifier, 0.2-3 parts of initiator, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide.
2. The antibacterial and antiviral acrylic emulsion according to claim 1, wherein the rare earth micropowder is one or both of boron molybdate crystals of lanthanide rare earth and iron oxide crystals of lanthanide rare earth.
3. The antibacterial and antiviral acrylic emulsion as claimed in claim 1, wherein said rare earth micropowder is a crystalline micropowder having a particle size of not more than 120 nm.
4. The acrylic emulsion according to claim 1, wherein the silver ion solution is a silver-based antibacterial agent.
5. The antibacterial and antiviral acrylic emulsion according to claim 1, wherein said emulsifier is composed of an anionic emulsifier and a nonionic emulsifier.
6. The antibacterial and antiviral acrylic emulsion according to claim 5, wherein said anionic emulsifier is one or both of sodium alkyl sulfate and sodium alkyl sulfonate.
7. The antibacterial and antiviral acrylic emulsion as claimed in claim 5, wherein said nonionic emulsifier is alkyl alcohol polyoxyethylene ether containing 9-11 EO.
8. The antibacterial and antiviral acrylic emulsion according to claim 1, wherein said initiator is one or more of ammonium persulfate, potassium persulfate and sodium persulfate.
9. The method for preparing an antibacterial and antiviral acrylic emulsion as claimed in any one of claims 1 to 8, comprising the steps of:
s001, preparing a base material liquid A: adding 40-50 parts of deionized water, 0-5 parts of emulsifier and all rare earth micro powder into a reaction kettle with a stirring device, a condensing device and a constant flow pump feeding device, stirring, heating to make the temperature in the reaction kettle reach 60-90 ℃, keeping the temperature and continuously stirring to prepare a bottom feed liquid A for later use;
s002, preparing a pre-emulsion B: adding 40-50 parts of deionized water, 1-8 parts of emulsifier, 0-20 parts of isooctyl acrylate, 0-60 parts of butyl acrylate, 10-45 parts of methyl methacrylate, 0.2-2.5 parts of acrylic acid, 0-2 parts of methacrylic acid, 0.2-2.5 parts of acrylamide and 0-2 parts of methacrylamide into an emulsifying cylinder with a metering device and a stirring device at normal temperature and normal pressure, stirring and mixing to obtain a uniform pre-emulsion B, and stirring for later use;
s003, preparing an initiator solution C: adding the rest deionized water and 0.2-3 parts of initiator into an initiator cylinder with a stirring device and a constant-current dropping device at normal temperature and normal pressure, and stirring until the deionized water and the initiator are completely dissolved for later use;
s004, when the temperature in the reaction kettle reaches 60-90 ℃, adding 4-10% of the total amount of the pre-emulsion B and 20-50% of the total amount of the initiator solution C into the bottom material solution A in the reaction kettle, reacting for 5-30 minutes, then simultaneously dropwise adding the rest of the pre-emulsion B and the rest of the initiator solution C into the reaction kettle through a constant flow pump feeding device and a constant flow dropwise adding metering device, controlling the dropwise adding time to be 150-240 minutes, and finishing dropwise adding the initiator solution C0-30 minutes later than the pre-emulsion B;
s005, controlling the temperature in the reaction kettle to be 60-90 ℃, preserving the heat for 1-2 hours, then cooling, adjusting the pH of the emulsion to be 7.0-9.0 by using an ammonia water solution, stirring for 0.5 hour, then adding all silver ion solutions, stirring for 0.5 hour, filtering and discharging to obtain the antibacterial and antiviral acrylic emulsion.
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Cited By (6)
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| CN114634603A (en) * | 2022-04-16 | 2022-06-17 | 濮阳林氏医疗制品有限公司 | Antibacterial inorganic-organic dispersion liquid and preparation method and application thereof |
| WO2022176743A1 (en) * | 2021-02-18 | 2022-08-25 | 共同印刷株式会社 | Fungicide, fungicide product, and fungicidal coating |
| WO2022176742A1 (en) * | 2021-02-18 | 2022-08-25 | 共同印刷株式会社 | Antimicrobial agent, antimicrobial product, and antimicrobial coating |
| WO2023090291A1 (en) * | 2021-11-16 | 2023-05-25 | 共同印刷株式会社 | Antiviral agent, antiviral product, and antiviral treatment liquid |
| WO2023210697A1 (en) * | 2022-04-28 | 2023-11-02 | 共同印刷株式会社 | Rare earth ferrite particles and rare earth ferrite dispersion liquid |
| WO2023210588A1 (en) * | 2022-04-28 | 2023-11-02 | 共同印刷株式会社 | Rare earth ferrite particle and rare earth ferrite dispersion liquid |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2022176743A1 (en) * | 2021-02-18 | 2022-08-25 | 共同印刷株式会社 | Fungicide, fungicide product, and fungicidal coating |
| WO2022176742A1 (en) * | 2021-02-18 | 2022-08-25 | 共同印刷株式会社 | Antimicrobial agent, antimicrobial product, and antimicrobial coating |
| WO2023090291A1 (en) * | 2021-11-16 | 2023-05-25 | 共同印刷株式会社 | Antiviral agent, antiviral product, and antiviral treatment liquid |
| CN114634603A (en) * | 2022-04-16 | 2022-06-17 | 濮阳林氏医疗制品有限公司 | Antibacterial inorganic-organic dispersion liquid and preparation method and application thereof |
| CN114634603B (en) * | 2022-04-16 | 2023-09-22 | 濮阳林氏医疗制品有限公司 | Antibacterial inorganic-organic dispersion liquid and preparation method and application thereof |
| WO2023210697A1 (en) * | 2022-04-28 | 2023-11-02 | 共同印刷株式会社 | Rare earth ferrite particles and rare earth ferrite dispersion liquid |
| WO2023210588A1 (en) * | 2022-04-28 | 2023-11-02 | 共同印刷株式会社 | Rare earth ferrite particle and rare earth ferrite dispersion liquid |
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