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WO2023012765A1 - Composition biocide et son procédé de préparation - Google Patents

Composition biocide et son procédé de préparation Download PDF

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Publication number
WO2023012765A1
WO2023012765A1 PCT/IB2022/057365 IB2022057365W WO2023012765A1 WO 2023012765 A1 WO2023012765 A1 WO 2023012765A1 IB 2022057365 W IB2022057365 W IB 2022057365W WO 2023012765 A1 WO2023012765 A1 WO 2023012765A1
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Prior art keywords
range
monomer
composition
predetermined
group
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English (en)
Inventor
Srikrushna PATNAIK
Vijay Chintaman KARANDIKAR
Dhiresh Shashikant GOSALIA
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Jesons Industries Ltd
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Jesons Industries Ltd
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Publication of WO2023012765A1 publication Critical patent/WO2023012765A1/fr
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Classifications

    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
    • A01P1/00—Disinfectants; Antimicrobial compounds or mixtures thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
    • A01N25/08—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing solids as carriers or diluents
    • A01N25/10—Macromolecular compounds
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
    • A01N33/02—Amines; Quaternary ammonium compounds
    • A01N33/12—Quaternary ammonium compounds

Definitions

  • the present disclosure relates to a biocidal composition and a process for its preparation.
  • Minimum film forming temperature refers to a lowest temperature at which an emulsion will uniformly coalesce when laid on a substrate as a thin film. An accurate minimum film forming temperature value allows the formulation of products that cure correctly under specified application conditions.
  • Open time refers to a period of time during which irregularities in a freshly applied coating can be repaired.
  • a cationic monomer is incorporated while designing the coating composition, which forms an integral part of coating composition.
  • the cationic surfactants such as cetylpyridinium chloride, cetylpyridinium bromide, dialkyl ammonium chloride, and like are added in the surface coating compositions.
  • suitable cationic compounds such as substituted pyridinium salts, substituted guanidine salts, tetrasubstituted ammonium salts and the like is incorporated during the coating preparation process.
  • incorporation of such cationic compounds in the final coating formulation is widely adopted to achieve anti-microbial efficacy.
  • leaching of the cationic compounds over a time period limits the performance of coating composition, with respect to its anti-microbial activity in a long run.
  • the use of such cationic compounds shows the anti-microbial efficacy for maximum of 3-4 months.
  • combining the cationic surfactant or any cationic molecules during the coating preparation process de-stabilizes the composition due to stringent processing conditions.
  • an inorganic material is combined with the final surface coating formulation.
  • the most commonly used inorganic material is based on silver ion and its nanoparticles. These silver ion or nanoparticles interact with sodium ion present in the microbes making them inactive.
  • the other metals, which have been explored as anti-microbial agents in the coating compositions are copper, copper oxide, zinc oxide and carbon black. However, the anti-microbial effect of these metal oxides is not persisting for longer period because of deactivation and leaching of nano-particles from the coated surface.
  • Another object of the present disclosure is to provide a biocidal composition.
  • Still another object of the present disclosure is to provide a biocidal composition, which is suitable for coating.
  • Another object of the present disclosure is to provide a biocidal composition, which is stable. Yet another object of the present disclosure is to provide a process for the preparation of the biocidal composition.
  • Still another object of the present disclosure is to provide a surface coating composition.
  • Another object of the present disclosure is to provide a surface coating composition, which is stable at least for 24 months.
  • the present disclosure provides a biocidal composition.
  • the composition comprising a homogenous mixture of: a polymer backbone, 0.1 to 5% of a plurality of additives, 0.1 to 1% of a biocide, 0.2 to 0.6% of a neutralizer, and 40 to 55% of water.
  • the polymer backbone comprises 1 to 5% of at least one cationic monomer, 10 to 30% of at least one alkyl acrylate monomer, 1 to 3% of at least one alkyl methacrylate monomer, 10 to 25% of at least one styrene monomer, 0.1 to 1% of at least one ureido monomer, and 1 to 5% of at least one cross-linking monomer.
  • the additives are selected from the group consisting of a methacryloxy silane, an epoxy silane oligomer, and a non-ionic surfactant.
  • the at least one of the additives being the non-ionic surfactant.
  • the present disclosure further provides a process for preparing a biocidal composition.
  • predetermined amounts of at least one alkyl acrylate monomer, at least one alkyl methacrylate monomer, at least one cationic monomer, at least one first non- ionic surfactant, at least one styrene monomer, at least one ureido monomer, and at least one cross-linking monomer are added in water under stirring at a first predetermined stirring speed, at a first predetermined temperature for a first predetermined time period to obtain a pre-emulsion slurry.
  • predetermined amounts of at least one second non-ionic surfactant and water are mixed in a second reactor under stirring at a second predetermined stirring speed, at a second predetermined temperature for a second predetermined time period to obtain a first mixture.
  • the pre-emulsion slurry is then added to the first mixture in a first predetermined ratio to obtain a second mixture.
  • a predetermined amount of a first catalyst is added to the second mixture followed by reacting at a third predetermined temperature for a third predetermined time period under stirring at a third predetermined stirring speed in the second reactor to obtain a first reaction mixture.
  • a predetermined amount of a second catalyst is added to the first reaction mixture followed by reacting at a fourth predetermined temperature for a fourth predetermined time period under stirring at a fourth predetermined stirring speed to obtain a second reaction mixture.
  • predetermined amounts of a neutralizer, a biocide and a plurality of additives are added in water to obtain a third mixture.
  • the additives are selected from the group consisting of methacryloxy silane, an epoxy silane oligomer, and a third non-ionic surfactant. At least one of the additives being the third non-ionic surfactant.
  • the third mixture is mixed to the second reaction mixture followed by cooling to a temperature in the range of 25 to 35 °C to obtain the biocidal composition in the form a homogeneous mixture.
  • the present disclosure further provides a surface coating composition. It comprises 20 to 25 % of the biocidal composition, 0.05 to 0.15% water softening agent, 0.60 to 1.0% dispersing agent, 0.4 to 0.8% wetting agent, 0.8 to 1.2% open time enhancer, 0.1 to 0.3% defoamer, 0.1 to 0.3% neutralizer, 0.1 to 0.5% cellulose thickner, 8 to 10% pigment, 30 to 35% extender, 0.6 to 1.0% preservatives, 0.2 to 0.6% adhesion promoters, 6 to 10% opaque polymer, 0.5 to 1.5% coalescing agent, and 18 to 22% water. All the percentages are with respect to the total weight of the surface coating composition.
  • Figure 1 illustrates a graph of log number of viral particles/percentage viral reduction vs time for the surface coating composition having biocidal composition of trial 1-12 (styrene based).
  • Figure 2 illustrates a graph of log number of viral particles/percentage viral reduction vs time for the surface coating composition having biocidal composition of trial 13-14 (pure acrylic based).
  • Embodiments are provided so as to thoroughly and fully convey the scope of the present disclosure to the person skilled in the art. Numerous details are set forth, relating to specific components, and methods, to provide a complete understanding of embodiments of the present disclosure. It will be apparent to the person skilled in the art that the details provided in the embodiments should not be construed to limit the scope of the present disclosure. In some embodiments, known processes or well-known apparatus or structures, and well known techniques are not described in detail.
  • first, second, third, etc. should not be construed to limit the scope of the present disclosure as the aforementioned terms may be only used to distinguish one element, component, region, layer or section from another component, region, layer or section. Terms such as first, second, third etc., when used herein do not imply a specific sequence or order unless clearly suggested by the present disclosure.
  • the conventional surface coating compositions which are used for anti-microbial applications extensively utilizes positively charged surfactants.
  • the limitation while using positively charged surfactant is that it leaches out with time when the surface coating is exposed to external environment, and therefore the efficacy of the surface coating composition decreases with time.
  • the preparation of surface coating compositions is very critical because of its instability in the surface coatings in long term.
  • the present disclosure provides a biocidal composition that would address the above described problem.
  • the present disclosure provides a biocidal composition.
  • the composition comprising a homogenous mixture of: a polymer backbone, a plurality of additives, a biocide, a neutralizer and water.
  • the polymer backbone comprises at least one cationic monomer, at least one alkyl acrylate monomer, at least one alkyl methacrylate monomer, at least one styrene monomer, at least one ureido monomer, and at least one crosslinking monomer.
  • the at least one cationic monomer is selected from the group consisting of diallyl dimethyl ammonium chloride, methacryloxy ethyl trimethyl ammonium chloride, acryloxy ethyl trimethyl ammonium chloride, vinyltrimethoxy silane, gamma-methacryloxypropyltrimethoxy silane, and dimethyl aminoethyl acrylate.
  • the cationic monomer is a combination of diallyl dimethyl ammonium chloride and vinyltrimethoxy silane.
  • the cationic monomer is a combination of diallyl dimethyl ammonium chloride and gammamethacryloxypropyltrimethoxy silane.
  • the cationic monomer is a combination of methacryloxy ethyl trimethyl ammonium chloride and vinyltrimethoxy silane. In still another exemplary embodiment, the cationic monomer is a combination of methacryloxy ethyl trimethyl ammonium chloride and gammamethacryloxypropyltrimethoxy silane. In still another exemplary embodiment, the cationic monomer is a combination of acryloxy ethyl trimethyl ammonium chloride and vinyltrimethoxy silane. In still another exemplary embodiment, the cationic monomer is a combination of acryloxy ethyl trimethyl ammonium chloride and gammamethacryloxypropyltrimethoxy silane .
  • the amount of at least one cationic monomer is in the range of 1 to 5% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of cationic monomer is 3% with respect to the total weight of the biocidal composition.
  • the alkyl acrylate monomer is selected from the group consisting of butyl acrylate, ethyl acrylate, 2-ethyl hexyl acrylate, n-butyl methacrylate.
  • the alkyl acrylate monomer is butyl acrylate.
  • the alkyl acrylate is ethyl acrylate.
  • the alkyl acrylate is 2-ethyl hexyl acrylate.
  • the amount of the alkyl acrylate monomer is in the range of 10 to 30% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the alkyl acrylate monomer is 18%. In another exemplary embodiment, the amount of alkyl acrylate monomer is 23%.
  • the alkyl methacrylate monomer is selected from the group consisting of methyl methacrylate, ethyl methacrylate, and butyl methyl acrylate.
  • the alkyl acrylate is methyl methacrylate.
  • the alkyl acrylate is ethyl methacrylate.
  • the alkyl methacrylate monomer is butyl methyl acrylate.
  • the amount of alkyl methacrylate monomer is in the range of 1 to 3% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the alkyl methacrylate monomer is 2% with respect to the total weight of the biocidal composition.
  • the amount of styrene monomer is in the range of 10 to 25% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the styrene monomer is 20%. In another exemplary embodiment, the amount of the styrene monomer is 15%.
  • the ureido monomer is N-(2- Methacryloyloxyethyl)-ethylene urea.
  • the amount of ureido monomer is in the range of 0.1 to 1 % with respect to the total weight of the composition. In an exemplary embodiment, the amount of ureido monomer is 0.5% with respect to the total weight of the biocidal composition.
  • the cross-linking monomer is selected from the group consisting of ethylene glycol dimethacrylate, and N-methylol acrylamide.
  • the cross-linking monomer is a combination of ethylene glycol dimethacrylate and 50% acrylamide.
  • the amount of the cross-linking monomer is in the range of 1 to 5% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of cross-linking monomer is 2.5% with respect to the total weight of the biocidal composition.
  • the additives are selected from the group consisting of a methacryloxy silane, and an epoxy silane oligomer.
  • the additive is an epoxy silane oligomer.
  • the at least one of the additives being a non-ionic surfactant.
  • the amount of the plurality of additives are in the range of 0.1% to 10%. In an exemplary embodiment, the amount of additives is 1 % with respect to the total weight of the biocidal composition.
  • the non-ionic surfactant is fatty alcohol ethoxylate having an ethylene oxide mol in the range of 20 to 40 mol. In an exemplary embodiment, the non-ionic surfactant is fatty alcohol ethoxylate having 40 mol ethylene oxide. In another exemplary embodiment, the non-ionic surfactant is fatty alcohol ethoxylate having 30 mol ethylene oxide. In still another exemplary embodiment, the non-ionic surfactant is fatty alcohol ethoxylate having 20 mol ethylene oxide.
  • the biocide is selected from the group consisting of 2,2 dibromo-3-nitrilopropionamide (Bruggolite), and disodium octaborate tetrahydrate.
  • the biocide is a combination of 2,2 dibromo-3-nitrilopropionamide and disodium octaborate tetrahydrate.
  • the amount of the biocide is in the range of 0.1 % to 1 % with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the biocide is 0.5% with respect to the total weight of the biocidal composition.
  • the neutralizer is selected from the group consisting of liquid ammonia, sodium hydroxide, potassium hydroxide and ammonium hydroxide.
  • the neutralizer is liquid ammonia.
  • the amount of neutralizer is in the range of 0.2 to 0.6% with respect to total weight of the biocidal composition. In an exemplary embodiment, the amount of neutralizer is 0.4% with respect to the total weight of the biocidal composition.
  • the biocidal composition is characterized by having solids in the range of 40 wt. % to 60 wt. %. In an exemplary embodiment, the biocidal composition has 45.5% of solid. The solids have a particle size is in the range of 200 nm to 250 nm.
  • the biocidal composition of the present disclosure has a pH in the range of 7 to 9.
  • the biocidal composition of the present disclosure has a viscosity in the range of 0.1 poise to 3.0 poise at 30 °C.
  • the biocidal composition of the present disclosure has a minimum film forming temperature is in the range of 16 °C to 22 °C.
  • the biocidal composition is cationic.
  • the biocidal composition is in the form of an emulsion.
  • the composition of the present disclosure is suitable for application in paints, textiles and paper coating.
  • the cationic monomers of the composition of the present disclosure which are added in minimal quantities, have the functionality which can contribute to anti-microbial performance. They are covalently attached to the polymer in order to have long term effect as long as the paint or coating remains on the substrate.
  • the prepared biocidal composition is very stable when formulated with paint or coatings, which is crucial to achieve.
  • the biocidal composition when mixed with paint/coating shows antibacterial and antiviral activity. The extended efficacy is observed when exposed to envelop viruses such as H1N1 and H3N2.
  • the biocidal composition of the present disclosure is designed with non-ionic surfactant instead cationic surfactant which provides stability to the paint and coating system.
  • the biocidal composition of the present disclosure is styrene based, which improves the antiviral activity when mixed with paints or coatings.
  • the biocidal composition of the present disclosure is long acting and suitable for coating.
  • the biocidal composition comprises a homogeneous mixture of a polymer backbone, 1 to 3% of a plurality of additives, 0.2 to 0.8% of a biocide, 0.2 to 0.6% of a neutralizer; and 40 to 55% of water. All the percentages are with respect to the total weight of the biocidal composition.
  • the polymer backbone comprises 3 to 4% of at least one cationic monomer, 15 to 25% of at least one alkyl acrylate monomer, 1.5 to 2.5% of at least one alkyl methacrylate monomer, 13 to 23% of at least one styrene monomer, 0.2 to 0.7% of at least one ureido monomer, and 2 to 3% of at least one cross-linking monomer.
  • the additives are selected from the group consisting of methacryloxy silane, an epoxy silane oligomer, and a non-ionic surfactant; and at least one of the additives are the non-ionic surfactant;
  • the present disclosure provides a biocidal coat comprising a biocidal composition and a paint.
  • a ratio of the biocidal composition to the paint is in the range of 1:2 to 1:4.
  • the present disclosure further provides a process for preparing the biocidal composition.
  • a predetermined amount of at least one alkyl acrylate monomer, at least one alkyl methacrylate monomer, at least one cationic monomer, a first non-ionic surfactant, at least one styrene monomer, at least one ureido monomer, and at least one cross-linking monomer are added in water under stirring at a first predetermined stirring speed, at a first predetermined temperature for a first predetermined time period to obtain a pre-emulsion slurry.
  • the amount of the alkyl acrylate monomer is in the range of 10 to 30% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the alkyl acrylate monomer is 18%. In another exemplary embodiment, the amount of alkyl acrylate monomer is 23%
  • the amount of alkyl methacrylate monomer is in the range of 1 to 3% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the alkyl methacrylate monomer is 2% with respect to the total weight of the biocidal composition. In accordance with the present disclosure, the amount of at least one cationic monomer is in the range of 1 to 5% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of cationic monomer is 3% with respect to the total weight of the biocidal composition.
  • the amount of styrene monomer is in the range of 10 to 25% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of the styrene monomer is 20%. In another exemplary embodiment, the amount of the styrene monomer is 15%.
  • the amount of ureido monomer is in the range of 0.1 to 1% with respect to the total weight of the composition. In an exemplary embodiment, the amount of ureido monomer is 0.5% with respect to the total weight of the biocidal composition.
  • the amount of the cross-linking monomer is in the range of 1 to 5% with respect to the total weight of the biocidal composition. In an exemplary embodiment, the amount of cross-linking monomer is 2.5% with respect to the total weight of the biocidal composition.
  • the first predetermined stirring speed is in the range of 100 rpm to 250 rpm; the first predetermined temperature is in the range of 25 to 35 °C; and the first predetermined time period is in the range of 5 to 15 minutes.
  • the first predetermined stirring speed is 140 rpm; the first predetermined temperature is 30 °C; and the first predetermined time period is 10 minutes.
  • predetermined amounts of at least one second non-ionic surfactant and water are mixed under stirring at a second predetermined stirring speed, at a second predetermined temperature for second predetermined time period to obtain a first mixture.
  • the predetermined amount of second non-ionic surfactant is in the range of 1 to 5% with respect to total weight of the first mixture. In an exemplary embodiment, the predetermined amount of second non-ionic surfactant is 2.5%.
  • the second predetermined stirring speed is in the range of 100 to 250 rpm; the second predetermined temperature is in the range of 25 to 40 °C; and the second predetermined time period is in the range of 10 to 25 minutes.
  • the second predetermined stirring speed is 150 rpm; the second predetermined temperature is 35 °C; and the second predetermined time period is 20 minutes.
  • the pre-emulsion slurry is then added to the first mixture in a predetermined ratio to obtain a second mixture.
  • predetermined ratio of the pre-emulsion slurry to the first mixture is in the range of 1 to 4. In an exemplary embodiment, the predetermined ratio of the pre-emulsion slurry to the first mixture is 2.6.
  • a predetermined amount of a first catalyst is then added to the second mixture followed by reacting at a third predetermined temperature for a third predetermined time period under stirring at a third predetermined stirring speed, to obtain a first reaction mixture.
  • the predetermined amount of the first catalyst is in the range of 0.5 to 5% with respect to the total weight of the second mixture. In an exemplary embodiment, the predetermined amount of the first catalyst is 2% with respect to the total weight of the second mixture.
  • the third predetermined stirring speed is in the range of 100 rpm to 300 rpm; the third predetermined temperature is in the range of 50 to 70 °C; and the third predetermined time period is in the range of 2.5 to 4.0 h.
  • the third predetermined stirring speed is 180 rpm; the third predetermined temperature is 55 °C; and the third predetermined time period is 10 minutes.
  • a predetermined amount of a second catalyst is added to the first reaction mixture followed by reacting at a fourth predetermined temperature for a fourth predetermined time period under stirring at a fourth predetermined stirring speed to obtain a second reaction mixture.
  • the predetermined amount of the second catalyst is in the range of 8 to 18% with respect to the weight of the first reaction mixture. In an exemplary embodiment, the predetermined amount of the second catalyst is 15% with respect to total weight of the first reaction mixture.
  • the fourth predetermined stirring speed is in the range of 100 to 250 rpm; the fourth predetermined temperature is in the range of 50 to 70 °C; and the fourth predetermined time period is in the range of 5 to 15 minutes. In an exemplary embodiment, the fourth predetermined stirring speed is 150-200 rpm; the fourth predetermined temperature is 55 °C; the fourth predetermined time period is 10 minutes.
  • a neutralizer e.g., a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate, a sulfate,
  • the neutralizer is at least one selected from the group consisting of liquid ammonia, sodium hydroxide, potassium hydroxide, and ammonium hydroxide.
  • the neutralizer is liquid ammonia.
  • the predetermined amount of neutralizer is in the range of 0.2 to 0.6% with respect to total weight of the biocidal composition. In an exemplary embodiment, the predetermined amount of neutralizer is 0.5% with respect to the total weight of the biocidal composition.
  • the biocide is selected from the group consisting of 2,2 dibromo- 3 -nitrilopropionamide (Mergal 530), and disodium octaborate tetrahydrate.
  • the biocide is a combination of 2,2 dibromo- 3- nitrilopropionamide and disodium octaborate tetrahydrate.
  • the predetermined amount of biocide is in the range of 0.1 to 1 % with respect to total weight of the biocidal composition. In an exemplary embodiment, the predetermined amount of biocide is 0.5% with respect to the total weight of the biocidal composition.
  • the biocidal composition is stable at least for three months.
  • the predetermined amount of additives is in the range of 0.1 to 5% with respect to total weight of the biocidal composition. In an exemplary embodiment, the predetermined amount of additives is 1% with respect to the total weight of the biocidal composition.
  • the third mixture is added to the second reaction mixture followed by cooling to a temperature in the range of 25 to 35 °C to obtain the biocidal composition in the form a homogeneous mixture.
  • the first catalyst is a mixture of 0.1 to 0.3% of an activator, 0.1 to 0.3% of a chelating agent, 0.01 to 0.05% of a first reducing agent, 0.01 to 0.05% of a first oxidizing agent, 0.005 to 0.01% of a fourth non-ionic surfactant and 0.5 to 2 % of water.
  • the activator is iron sulphate.
  • the chelating agent is ethylenediaminetetraacetic acid sodium salt.
  • the second catalyst is a mixture of 0.1 to 0.5% a second reducing agent, 0.5 to 2% of a second oxidizing agent, 0.05 to 0.2% of a fifth non-ionic surfactant, and 8 to 13% of water.
  • the first oxidizing agent and the second oxidizing agent are same or different and are independently selected from persulphate and peroxide.
  • the persulphate is selected from the group consisting of potassium persulphate, sodium persulphate, and ammonium persulphate.
  • the peroxide is selected from the group consisting of tertiary butyl hydroperoxide, hydrogen peroxide, and benzoyl peroxide.
  • the oxidizing agent is tertiary butyl hydroperoxide.
  • the first reducing agent and the second reducing agent are same or different and are independently selected from sodium formaldehyde sulphoxylate, sodium acetone, sodium meta bisulphite, sodium hydroxymethylsulfinate (Bruggolite), and sodium acetone bisulphite.
  • the first reducing agent is a combination of sodium hydroxymethylsulfinate (Bruggolite) and sodium acetone bisulphite.
  • the second reducing agent is a combination of sodium hydroxymethylsulfinate (Bruggolite) and sodium acetone bisulphite.
  • a weight ratio of the first/second oxidizing agent to the first/second reducing agent is in the range of 0.05% to 2%.
  • At least one second cationic monomer, a biocide, a third non-ionic surfactant and at least one neutralizer are mixed with water to obtain a mixture.
  • the mixture is then mixed with the second reaction mixture to obtain the biocidal composition.
  • the first non-ionic surfactant, the second non-ionic surfactant, the third non-ionic surfactant, the fourth non-ionic surfactant, and the fifth non- ionic surfactant are same or different and are independently selected from fatty alcohol ethoxylate having ethylene oxide in the range 20 mol to 40 Mol.
  • the process of the present disclosure is a redox process rather conventional process.
  • the redox process incorporates less reactive but better performing specialty cationic monomers in the polymer backbone.
  • the combination of cationic monomer and ureido monomer plays a significant role in providing antimicrobial activity along with better adhesion of paint/coating to the substrate.
  • the prepared paints and coatings show above 99 % efficacy to antibacterial and antiviral application and at the same to envelop viruses such as H1N1 and H3N2.
  • the monomers are fully polymerized.
  • the present disclosure further provides a surface coating composition.
  • the surface coating composition comprises 20 to 25% of a biocidal composition of the present disclosure, 0.05 to 0.15% water softening agent, 0.60 to 1.0% dispersing agent, 0.4 to 0.8% wetting agent, 0.8 to 1.2% open time enhancer, 0.1 to 0.3% defoamer, 0.1 to 0.3% neutralizer, 0.1 to 0.5% cellulose thickner, 8 to 10% pigment, 30 to 35% extender, 0.6 to 1.0% preservatives, 0.2 to 0.6% adhesion promoters, 6 to 10% opaque polymer, 0.5 to 1.5% coalescing agent, and 18 to 22% water. All the percentages are with respect to the total weight of the surface coating composition.
  • the water softening agent is selected from the group consisting of tetrasodium pyrophosphate and ethylene diamine tetra acetic acid.
  • the water softening agent is tetrasodium pyrophosphate.
  • the dispersing agent is selected from the group consisting of a polyacrylate having a molecular weight in the range of 1000 to 7000 Da.
  • the dispersing agent is a poly aery late having a molecular weight ⁇ 5000 Da (Bondex 532).
  • the wetting agent is selected from the group consisting of alkyl phenol ethoxylate.
  • the wetting agent is nonyl phenol 40 mol ethoxylate (IG Surf 8405).
  • the open time enhancer is a glycol.
  • the open time enhancer is triethylene glycol.
  • the defoamer is selected from the group consisting of mineral oil, polyether, silica and a mixture thereof.
  • the defoamer is a mixture of mineral oil, polyether and silica (San Napco SN 1370).
  • the neutralizer is 95% aqueous solution of 2-amino-2-methyl-l -propanol (AMP 95).
  • the thickener is selected from the group consisting of water soluble non-ionic hydroxyethylcellulose and associative polyurethane.
  • the thickner is a mixture of water soluble non-ionic hydroxyethylcellulose (Natrosol 250 HBR) and associative polyurethane (Rheolite 99).
  • the pigment is selected from the group consisting of rutile TiCK
  • the extender is selected from the group consisting of CaCCh. calcined kaolin, talc powder and a mixture thereof.
  • the extender is a mixture of CaCCh. calcined kaolin and talc powder.
  • the preservative is benzimidazole carbamate. In an exemplary embodiment, the preservative is Acticide EPW 1.
  • the adhesion promoter is 3-(2,3- epoxypropoxypropyl)methyldiethoxysilane. In an exemplary embodiment, the adhesion promoter is 3-(2,3-epoxypropoxypropyl)methyldiethoxysilane (Wetlink 78).
  • the opaque polymer is Bondex Opex 90 (styrene based).
  • the coalescing agent is a film former selected from texanol and butylcarbitol.
  • the coalescing agent (film former) is texanol.
  • the biocidal composition acts as a binder.
  • the viscosity of the surface coating composition of the present disclosure is in the range of 25 to 35 poise. In an exemplary embodiment, the viscosity of the surface coating composition is 28.4 poise.
  • the present disclosure provides a method for treating a surface for biocidal activity.
  • the surface is selected from the group consisting of internal wall surface, internal ceiling surface, external wall surface, and external roof surface.
  • the surface is internal wall surface.
  • a primer coat is applied on the surface and the primer is allowed to dry to obtain a primer coated surface.
  • a coat having a uniform thickness in the range of 200 microns to 500 microns is applied on the primer coated surface to obtain a coated surface.
  • the coat is carried out by using at least one composition selected from the biocidal composition of the present disclosure, the biocidal coat of the present disclosure, and the surface coating composition of the present disclosure.
  • the coat is applied by using at least one appliance selected from a brush and a roller.
  • the coated surface is cured for a time period in the range of 2 hours to 6 hours to obtain the treated surface.
  • the coated surface is cured for a time period in the range of 2 hours to 3 hours.
  • the treated surface has a dry film thickness in the range of 100 microns to 250 microns. In an embodiment of the present disclosure, the treated surface has a dry film thickness in the range of 100 microns to 150 microns.
  • the composition of the present disclosure is suitable for application in paints, textiles and paper coating.
  • the cationic monomers of the composition of the present disclosure which are added in minimal quantities, have the functionality which can contribute to anti-microbial performance. They are covalently attached to the polymer in order to have long term effect as long as the paint or coating remains on the substrate.
  • the prepared biocidal composition is very stable when formulated with paint or coatings, which is crucial to achieve.
  • the biocidal composition when mixed with paint/coating shows antibacterial and antiviral activity. The extended efficacy is observed when exposed to envelop viruses such as H1N1 and H3N2.
  • EXPERIMENTAL DETAILS Experiment 1: Process for preparing a long lasting biocidal composition in accordance with the present disclosure
  • a demineralized water was added in a second reactor.
  • a non-ionic surfactant (fatty alcohol ethoxylate) was added to water under stirring at a stirring speed of 150 rpm at 35 °C for 20 minute to obtain a first mixture.
  • Table 2 illustrates various combinations of fatty alcohol ethoxylate with demineralized water.
  • the pre-emulsion slurry was added to the first mixture in a ratio of 2.6 to obtain a second mixture.
  • 1.8 % of first catalyst (with respect to the total weight of second mixture) was added to the second mixture followed by reacting at 55 °C for 10 min under stirring at a stirring speed of 180 rpm (with respect to the weight of pre-emulsion slurry) to obtain a first reaction mixture.
  • 5 wt% of seed polymer was added with respect to the total weight of the pre- emulsion slurry to initiate the reaction.
  • Table 3 illustrates a composition of the first catalyst.
  • the second catalyst also refers to a delayed catalyst that is added slowly over the time period of 3 to 4 hr in the reactor.
  • Table 4 discloses a composition of the second catalyst.
  • a neutralizer liquid ammonia
  • a biocide Mergal 530 and disodium octaborate tetrahydrate
  • an additive epoxy silane oligomer and third non-ionic surfactant i.e. fatty alcohol ethoxylate
  • the third mixture was then mixed to the second reaction mixture followed by cooling to a temperature in the range of 25 to 35 °C to obtain the biocidal composition in the form a homogeneous mixture.
  • Table 5 represents the composition which is added after the polymerization reaction is finished.
  • the total weight in each of the trial T1-T14 was 1000 g.
  • the pH of the biocidal compositions of T1-T12 were in the range of 7-9.
  • the specific gravity of the biocidal compositions (T1-T12) were in the range of 1.02 to 1.09, as measured using ASTM 1475 (see table 6).
  • the amount of solid content of the biocidal composition (T1-T12) was 45 to 46%, as determined ASTM D 2369 (see table 6).
  • the viscosity of the biocidal compositions was measured using Brookfield RVT Spindle 2, speed 20 at 30 °C, was in the range of 1-2 poise (see table 6).
  • Example 4 Determination of minimum film forming temperature (MFFT) of the biocidal composition A standard test method ASTM D2354 was followed for determining MFFT of the biocidal composition.
  • the MFFT of the biocidal composition was found to be 18-20 °C (T1-T12). Below 18-20 °C, the biocidal composition did not form a continuous film and it cracks.
  • Table 2 illustration of various combinations of non-ionic surfactants with water to prepare the first mixture
  • Table 3 A composition of the first catalyst
  • Table 5 A composition of a third mixture for post-addition
  • the particle sizes of the solid particles were found to be in the range of 200 nm to 250 nm (T1-T12).
  • the biocidal composition was prepared as per experiment 1(T1-T12).
  • the surface coating composition was prepared by mixing 22 wt% of biocidal composition, 0.1 wt% of tetrasodium pyrophosphate (water softening agent), 0.8 wt% of Bondex 532 (dispersing agent), 0.6 wt% of IG Surf 8405 (wetting agent), 1.0 wt% of triethylene glycol (open time enhancer), 0.2 wt% of San Napco SN 1370 (defoamer), 0.2 wt% of AMP 95 (neutralizer), 0.3 wt% of Natrosol 250 HBR (thickner/cellulose thickner), 9% of Rutile TiCL R 902 (pigment), 17 wt% CaCCh, 12 wt% calcined kaolin, and 4 wt% talk powder 2 p (extenders), 0.20 wt% preventol (In can preservative), 0.6 wt% Acticide EPW 1 (dry film preservative), 0.40 wt% Wetlink 78
  • the viscosity of the surface coating composition was found to be 28.4 poise as measured using Brookfield viscometer with spindle 2 at 20 rpm and 30 °C.
  • the virus killing activity of the surface coating composition was commercially performed at Centre for Cellular and Molecular Biology Laboratory, Hyderabad, India.
  • the surface coating composition having 22 wt% of biocidal compositions which is styrene based was evaluated for the efficacy to kill corona virus (SARS_CoV2) when inoculated at a concentration of 1 x 10 7 viral particles per ml.
  • SARS_CoV2 corona virus
  • Table 7 Surface coating composition of the present disclosure (white paint @ 22% Bondex AMCAS 46-2)
  • the viral assay was performed using (i) viral RNA extraction method using MagMAXTM Viral/Pathogen Extraction Kit from Applied Biosystems (Thermo Fisher), and (ii) qRT-PCR using Q-line Molecular nCOV-19 RT-PCR Detection Kit (Multiplex) manufactured by POCT Services Private Limited. The assays were performed at 5 minute intervals. The experiments were performed in duplicates and the values were averaged to calculate % viral reduction.
  • the number of viral particles (x) were calculated using the following equation: — (40.786-CtRdrp.gene at different time points)/3-5442 (2)
  • the percentage of viral reduction was calculated using the following equation:
  • % viral reduction ((number of viral particles in infection control-number of viral particles exposed to surface (test))/(number of viral particles in infection control))* 100 (3)
  • the surface coating composition of the present disclosure showed -99% viral reduction from 25 minutes onward.
  • the viral particles number reduced from IxlO 6 ' 9 to IxlO 4 ' 3 (See figure 1).
  • the viral assay was performed using (i) viral RNA extraction method using MagMAXTM Viral/Pathogen Extraction Kit from Applied Biosystems (Thermo Fisher), and (ii) qRT-PCR using Meril Covid-19 one-step RT-PCR Kit from Meril Diagnostics Pvt. Ltd.
  • the percentage of viral reduction was calculated using equation (3).
  • the surface coating composition of the present disclosure showed -94% viral reduction from 45 minutes onward.
  • the viral particles number reduced from IxlO 5 ' 7 to IxlO 4 ' 4 (see figure 2). It was found that the surface coating composition prepared using biocidal composition of T1-T12 (styrene based) showed higher efficiency that those prepared using biocidal composition of T13-T14 (pure acrylic based).
  • the surface coating composition showed remarkable result in killing the virus on contact due to the cationic nature of the surface developed due to biocidal composition.
  • the proposition of killing virus was based on electrostatic force generated by the biocidal composition to the paint which attracts the negative charge virus and thus activated the same due to puncture of cell membrane, and deactived the protein layer.
  • One of the objects of the Patent Law is to provide protection to new technologies in all fields and domain of technologies.
  • the new technologies shall or may contribute in the country economy growth by way of involvement of new efficient and quality method or product manufacturing in India.
  • the applicant submits that the present disclosure will contribute in country economy, which is one of the purposes to enact the Patents Act, 1970.
  • the product in accordance with present invention will be in great demand in country and worldwide due to novel technical features of a present invention is a technical advancement in the surface coating technology.
  • the technology in accordance with present disclosure will provide product cheaper, saving in time of total process of manufacturing. The saving in production time will improve the productivity, and cost cutting of the product, which will directly contribute to economy of the country.
  • the product will contribute new concept in the surface coating compositions wherein patented process/product will be used.
  • the present disclosure will replace the whole concept of surface coating being used in this area from decades.
  • the product is developed in the national interest and will contribute to country economy.
  • the economy significance details requirement may be called during the examination. Only after filing of this Patent application, the applicant can work publically related to present disclosure product/process/method. The applicant will disclose all the details related to the economic significance contribution after the protection of invention.

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  • Life Sciences & Earth Sciences (AREA)
  • Wood Science & Technology (AREA)
  • General Health & Medical Sciences (AREA)
  • Plant Pathology (AREA)
  • Health & Medical Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Zoology (AREA)
  • Pest Control & Pesticides (AREA)
  • Environmental Sciences (AREA)
  • Agronomy & Crop Science (AREA)
  • Dentistry (AREA)
  • Toxicology (AREA)
  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • General Chemical & Material Sciences (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

La présente invention concerne une composition biocide et un procédé de préparation de celle-ci. La présente invention concerne également une composition de revêtement de surface. La composition biocide peut être utilisée dans une composition de revêtement de surface. La composition biocide comprend un squelette polymère, une pluralité d'additifs, un biocide, un neutralisant et de l'eau. La composition est préparée à l'aide d'une polymérisation redox. La composition peut tuer jusqu'à 99 % de virus H1N1 et H3N2, a un effet antimicrobien à long terme et est très stable lorsqu'elle est formulée avec la composition de revêtement de surface.
PCT/IB2022/057365 2021-08-06 2022-08-08 Composition biocide et son procédé de préparation Ceased WO2023012765A1 (fr)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011150001A2 (fr) * 2010-05-25 2011-12-01 3M Innovative Properties Company Revêtements antimicrobiens
EP2778195A1 (fr) * 2013-03-15 2014-09-17 Rohm and Haas Company Polymères redox pour une meilleure résistance à l'eau et à la saleté pour revêtements de paroi et toit élastomère
WO2020187606A1 (fr) * 2019-03-19 2020-09-24 Rhodia Operations Compositions biocides synergiques et procédés d'utilisation de celles-ci

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2011150001A2 (fr) * 2010-05-25 2011-12-01 3M Innovative Properties Company Revêtements antimicrobiens
EP2778195A1 (fr) * 2013-03-15 2014-09-17 Rohm and Haas Company Polymères redox pour une meilleure résistance à l'eau et à la saleté pour revêtements de paroi et toit élastomère
WO2020187606A1 (fr) * 2019-03-19 2020-09-24 Rhodia Operations Compositions biocides synergiques et procédés d'utilisation de celles-ci

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