Immobilised 1,2-benzisothiazolinone-3

FIELD: medicine, pharmaceutics.

SUBSTANCE: group of inventions refers to a method for preparing an immobilised 1,2-benzisothiazolin-3-one complex, an antimicrobial composition containing it and to using the above composition as an antimicrobial agent. The immobilised 1,2-benzisothiazolin-3-one is prepared by heating 1,2-benzisothiazolin-3-one and zinc chloride brought to the boiling point with partial condensation in C1-C4 alcohol to prepare a solution to be cooled and added with the immobilising effective amount of zinc oxide. The prepared mixture is brought to the boiling point with partial condensation, cooled to room temperature and filtered to prepare the immobilised 1,2 - benzisothiazolin-3-one/zinc oxide complex.

EFFECT: declared inventions provide producing the antimicrobial immobilised 1,2 - benzisothiazolin-3-one/zinc oxide complexes applicable as preserving agents due to their wash-out resistance.

12 cl, 4 dwg, 2 tbl, 22 ex

 

The scope of the invention

In the present invention proposed new antimicrobial complexes immobilized 1,2-benzothiazolin-3-one/zinc oxide, useful as preservatives due to their resistance to leaching from the substrate to which they are attached. The present invention also proposed a substrate having antimicrobial protection, including those that require high temperature processing, such as, but not limited to, powder coating, wood composites and plastics, such as polyvinyl chloride (PVC), low density polyethylene (LDPE), polyethylene of low density, plastisol, polyurethane.

Description of the prior art

Many of the materials that come in contact with moisture prone to the damaging effects of a number of microorganisms, including fungi, yeast, algae and bacteria. Therefore, there is a huge need for effective and economical means to protect such materials from such destructive effects over long periods of time. Commercial materials, which generally require such protection include, for example, plastics, wood, products of wood, wood composite materials, wood-plastic composite materials, injection molded plastics, construction materials, paper, toys, pokr is ment, materials based on proteins, compositions based on starch, inks, emulsions, resins, plaster, concrete, stone, wood adhesives, sealants, gaskets, leather, paints and varnishes for the skin, myliobatidae machines, packaging materials, paints for yarn, fabric, and rope products, basics carpeting, electrical insulation, medical devices, and the like.

In addition to commercial protective materials from such destructive effects it is also desirable to inhibit the growth of microorganisms on the surface of commercial materials to maintain hygienic conditions, for example, in hospitals, nurseries, institutions for the elderly, equipment for food industry, airplanes, trains, buses and the like.

No single antimicrobial compound does not protect against all micro-organisms or unsuitable for all applications. In addition to the restrictions regarding the effectiveness, other limitations include stability, physical properties, Toxicological profile, regulatory considerations, economic considerations and care about the environment. Antimicrobial agents that are suitable for many applications, may be unsuitable for other applications. Thus, there is a need to develop new PR is tuomikoski compositions which will provide protection for a variety of applications and under certain conditions to protect commercial materials from destructive effects of microorganisms and inhibiting the growth of microorganisms on the surface of commercial materials.

Widely used antimicrobial agent is 1,2-benzisothiazolin-3-one (BIT). BIT and its water-soluble salts of alkali metals are often the biocide of choice when industrial bactericide necessary to prevent microbial contamination of the technical water-based systems, such mineral suspensions, polymer emulsions, inks, paints, plaster mortars, adhesives and the like (see, for example, W. Paulus "Dictionary of Microbicides for the Protection of Materials pp.664-666 (2005), Springer, Dordrecht).

BIT and its salts are used primarily in liquid systems, as, for example, in the coatings industry (paints, varnishes and so on). BIT and its salts are used almost exclusively as preservatives for storage of paint in the container to protect the liquid paint while the paint is in the container before application and during application. BIT is not used to protect surfaces from microbial growth after it is deposited on the substrate, because the BIT is easily washed away from the dried film coating.

In U.S. patent No. 3065123 disclosed the addition of 1,2-benzisothiazolin-3-one in the aquatic environment C the shields of the aquatic environment from infection by microorganisms. In U.S. patent No. 4150026 disclosed complexes 3-isothiazolones with salts of metals which exhibit bactericidal, fungicidal and algaecidal properties. In U.S. patent No. 4188376 disclosed biocidal compositions suitable for use in indirect food contact and the storage of water-based paints in the container containing the solution of alkali metal salt of 1,2-benzisothiazolin-3-one in an alcohol, glycol or aqueous solvent. In U.S. patent No. 4871754 disclosed the use of aqueous preparations of the lithium salt of 1,2-benzisothiazolin-3-it is for the protection of aqueous solutions from infection by microorganisms.

Antimicrobial compounds that are effective as a film preservatives, such as Polyphase®the composition of 3-iodine-2-propynylbutylcarbamate remain in the dried coating and, therefore, can continue to protect this surface from microbial growth. Polyphase®effective mainly against fungi and mildew. Accordingly, there is a need for antibacterial film preservative with Toxicological profile BIT that does not lose its effectiveness over time due to evaporation or you-mevania (see W. Lindner "Chemisch-physikalisches Verhalten von Konservierungsmit-tel in Beschichtungsstoffen" (1998) Expert Verlag, Bd 509, W. Lindner in the "Directory of Microbicides for the Protection of Materials" (2005), W. Paulus (ed) Springer).

SUMMARY of the INVENTION

Nastojashem the invention proposed new Antimicrobial complexes immobilized 1,2-benzisothiazolin-3-one/zinc oxide (BIT/ZnO), useful as antimicrobial agents, which are resistant to leaching from the substrate to which they are attached. The present invention is also directed to methods for producing complexes of the BIT/ZnO, on complexes of the BIT/ZnO obtained by these new methods, methods using complexes BIT/ZnO for inhibiting microbial growth or reduce the level of bacteria on the surface of the substrate and on the substrate, protected from exposure to microbes as a result of processing complexes BIT/ZnO. The present invention also is directed to compositions containing 1,2-benzisothiazolin-3-one, which is immobilized zinc oxide.

A BRIEF DESCRIPTION of GRAPHIC MATERIALS

Figure 1 is a graph showing an infrared spectrum of 1,2-benzisothiazolin-3-one (BIT).

Figure 2 is a graph showing an infrared spectrum of zinc oxide (ZnO).

Figure 3 is a graph showing an infrared spectrum of the complex BIT/ZnO.

Figure 4 is a graph showing an infrared spectrum of the salt BITS/Li.

DETAILED description of the INVENTION

The inventors have made the discovery that the antimicrobial agent is 1,2-benzisothiazolin-3-one (BIT) can be immobilized by mixing this antimicrobial agent with immovable effective amount of zinc oxide (ZnO). Although they don't want to be is like any theory, the inventors believe that the antimicrobial agent and immovable agent are attracting interaction, which facilitates immobilization of antimicrobial agent from the generally harmful effects of leaching from the substrate to which it is applied. BITS and zinc oxide can form an acid-base complex, and additional zinc oxide may Deposit around the complex BIT/ZnO, because of the higher ratio of ZnO to BITS result in a higher propensity complex BIT/ZnO to immobilization. This immobilization delays or prevents the leaching of the antimicrobial agent and results in greater retention of antimicrobial protection in the target substrate than in the case where the immovable agent is not present. The combination of the antimicrobial agent and immovable agent unexpectedly acts as improving immobilization of antimicrobial agent on the substrate.

As shown in figures 1 to 4, the structure of the complex of the immobilized BIT/ZnO analyzed using infrared spectra. Figure 1 is a graph showing an infrared spectrum of BITS with a strong carbonyl band at 1645 cm-1. Figure 2 is a graph showing an infrared spectrum of ZnO. Figure 3 is a graph showing an infrared spectrum of the complex BITS/ZO. Figure 4 is a graph showing an infrared spectrum of the salt BITS/Li. The infrared spectrum of figure 3 clearly shows that the complex BIT/ZnO is not a physical mixture of BITS and ZnO as carbonyl band BITS at 1645 cm-1(1) absent. The complex of the immobilized BIT/ZnO is not a basic salt, which is evident in the comparison with the infrared spectrum of the salt BITS/Li (figure 4). One would expect that the infrared spectra of complex immobilized BIT/ZnO and salt BITS/Li must be very similar, since it involved the same organic anion. But the infrared spectra of complex immobilized BIT/ZnO and salt BITS/Li are different, mainly in the field of characteristic zones" from 700 cm-1up to 1400 cm-1, which represents the combined resonances of molecules BIT. In salt-BIT/Li stripes complex BIT/ZnO at 910, 899 and 797 cm-1missing, whereas in the complex BIT/ZnO stripes of salt BITS/Li at 1055 cm-1and 880 cm-1no. The infrared spectrum of ZnO (figure 2) is empty in the infrared range, present bands are the result of moisture (about 3300 cm-1or organic impurities in high concentration. The combination of infrared spectra in figure 1-4 together with HPLC analysis on a BIT, extracted with methanol, and the total BIT after hydrolysis (Note the market 2-7) suggests, that BIT must form a complex in ZnO.

BITS can be immobilized on the ZnO surfaces by deposition of water-soluble salts of BITS, in particular, alkali metal salts, for ZnO. Non-limiting examples of water-soluble zinc salts BITS include salts formed with zinc chloride, zinc bromide, zinc acetate, zinc formate and zinc nitrate. The method of obtaining complexes immobilized BIT/ZnO can be widely varied. Water-soluble salt of BITS can be precipitated on the surface of pre-formed zinc oxide by neutralizing the solution. For example, an aqueous solution of potassium salt of BITS can be mixed with ZnO and ZnCl2and then besiege BIT on ZnO by neutralizing the mixture. Alternative BITS and ZnO can be mixed directly with the formation of the BIT/ZnO. Additional zinc oxide can be precipitated on the pre-formed complexes of the BIT/ZnO. By selecting the conditions of deposition of the antimicrobial properties of the compounds can be varied. Complexes BIT/ZnO can be obtained in the form of solids or in the form of the dispersion concentrates using conventional dispersion techniques. The ratio of the masses/mass BIT to ZnO in the complex can be controlled so as to match the specific application of the final product. The particle size of the complex BIT/ZnO and viscosity to the Plex BIT/ZnO dispersion in the concentrate can also be adjusted so to match the specific application of the final product. Higher ratio of mass/mass ZnO BIT to result in greater susceptibility of the complex BIT/ZnO to immobilization. The particle size of the complex BIT/ZnO can be adjusted by grinding, and it can be in the range from nanoscale (about 10 nm) to several hundred microns. Typically, the complex is immobilized BIT/ZnO is deposited while the particle size, which is small enough to be directly used in the coating material. The viscosity of the dispersion concentrate complex BIT/ZnO can be adjusted by adding an agent regulating the viscosity. The preferred reaction medium is water, lower alcohols such as methanol, ethanol, isopropanol, n-propanol, n-butanol, ETOR-butanol, tert-butanol, and mixtures thereof. The complex of the immobilized BIT/ZnO can be distinguished using conventional techniques such as filtration or spray drying. The complex of the immobilized BIT/ZnO can be combined with additional antimicrobial agents and antifungal film preservatives, such as carbendazim (methylbenzimidazole-2-ylcarbamate), 3-iodine-2-propynylbutylcarbamate, pyrithione zinc, triclosan (5-chloro-2-(2,4-dichlorophenoxy)phenol), 2-n-acterization-3-one, 4,5-dichloro-2-n-acterization-3-one, CHLOROTHALONIL (2,4,5,6-tet is floridaflorida), beloxepin (3-benzo[b]Tien-2-yl-5,6-dihydro-1,4,2-oxathiazine 4-oxide), Zir (zinc bis(dimethyldithiocarbamate), thiram (Tetra-methylfuran disulfide), 2-n-butylbenzothiazole-3-one, as well as silver and silver compounds such as silver, is applied in the form of coating on zinc oxide AirQual AQ200, commercially available from the company AirQual, zinc compounds, silver zeolite, commercially available from the company Ciba, silver chloride on titanium dioxide, available in sales from the company Clariant, and silver (silver nanoparticles), commercially available from the company NANUX.

Antimicrobial complexes immobilized BIT/ZnO according to the present invention provide complex, where BIT is resistant to evaporation or leaching, or any other process that would have caused the depletion of BITS on the surface of the substrate. Antimicrobial complexes immobilized BIT/ZnO also provide antibacterial hygienic coatings for surfaces, such as in hospitals, nursing homes, kindergartens, devices for the food and pharmaceutical industry equipment. Bacteria that comes in contact with such surfaces, tempered by the presence of immobilized anti-bacterial agent. Such permanent Antimicrobial properties may provide procedures for cleaning and disinfection of hard surfaces. Antimicrobial immobile is organized complexes can also inhibit the formation of a film of microorganisms on the surface of materials for seals, as, for example, in water supply systems. Antimicrobial immobilized complexes provide additional antimicrobial compound, suitable for use in hygienic surfaces that should not be burdened with undesirable properties characteristic of other antimicrobial surfaces used for such purposes. Additional materials that can be coated with the antimicrobial complexes immobilized BIT/ZnO include coatings, plastics, wood products, wood composites, wood plastic composites, injection molding plastics, construction materials, paper, compositions based on starch, adhesives, plaster, concrete, sealants, gaskets, cloth and rope and rope products.

In accordance with the present invention, a method for obtaining complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide, which includes stages (a) heating 1,2-benzisothiazolin-3-one and zinc chloride to a boil with delegacia in C1-C4branched or unbranched alcohol to form a solution; (b) cooling of this solution and add immovable effective amount of zinc oxide to the solution with the formation of the mixture; (C) heating the mixture to a boil with delegacia, and then cooling the mixture to room t is mperature; (g) filtering the mixture to obtain complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide. This method may further include washing the solid substance, C1-C4branched or unbranched alcohol and drying the solid in vacuo. C1-C4branched or unbranched alcohols can be selected from the group consisting of methanol, ethanol, n-propanol, isopropanol, n-butanol, sec-butanol and tert-butanol. Preferably C1-C4branched or unbranched alcohols selected from the group consisting of methanol, ethanol, n-propanol and isopropanol, more preferably those alcohols are methanol or ethanol, and most preferably methanol.

In another embodiment of the present invention, a method for obtaining a dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide, which includes stages (a) education aqueous solution of 1,2-benzisothiazolin-3-one and potassium hydroxide having a pH from about 7 to about 8.5; (b) adding zinc chloride and immovable effective amount of zinc oxide to the solution with the formation of the mixture and (C) grinding the mixture with the formation of the dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide. This way is optional to include adding a dispersing agent to the mixture in stage (b) and inhibitor pricing to the mixture in stage (b).

In another embodiment of the present invention, a method for obtaining a dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide, which includes stages (a) formation of a water mixture of 1,2-benzisothiazolin-3-one, zinc chloride and immovable effective amount of zinc oxide; (b) bringing the pH of the mixture from about 7 to about 8.5, and (C) grinding the mixture with the formation of the dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide. This method may further include adding a dispersing agent to the mixture in stage (b) and a foaming inhibitor to the mixture in stage (b).

In another embodiment of the present invention, a method for obtaining a dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide, which includes stages (a) formation of a water mixture of 1,2-benzisothiazolin-3-one and immovable effective amount of zinc oxide and (b) grinding the mixture with the formation of the dispersion concentrate complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide. This method may further include adding a dispersing agent to the mixture in stage (a) and inhibitor pricing to the mixture in stage (b).

The present invention also proposed a complex immobilized 1,2-Ben is isothiazolin-3-one/zinc oxide received the above ways. In the present invention, furthermore, a method for protection of the substrate from contamination by microorganisms, in which process the substrate is effective against microorganisms number of complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide obtained above ways. In the present invention, in addition, the proposed composition containing 1,2-benzisothiazolin-3-one, which is immobilized zinc oxide.

The antimicrobial agent used in the complexes of immobilized BIT/ZnO according to the present invention, is a commercially available 1,2-benzisothiazolin-3-one (1,2-benzisothiazolin-3(2H)-he, BITS) and its salts. BIT has a molecular mass of 151,19, soluble in hot water and forms a water-soluble salts with alkali metals and amines, and also has a high solubility in organic solvents, in particular alcohols and glycols. BIT and its water-soluble salts of alkali metals useful to prevent microbial contamination of the technical water-based systems, such mineral suspensions, polymer emulsions, inks, paints, plaster mortars, adhesives and the like. BIT disclosed in U.S. patent No. 3065123, the description of which is incorporated herein by reference.

Immovable agent used in the complexes immobi savannaha BIT/ZnO according to the present invention, is a commercially available zinc oxide (ZnO). Zinc oxide has a molecular mass of 81,38, exists in the form of a white or yellowish-white powder, odorless and practically insoluble in water. You can also use the nanostructures of zinc oxide. Nanostructures of zinc oxide are described in detail in the publication Materialstoday, June (2004), pp.26-33, the description of which is incorporated herein by reference.

In accordance with the present invention immovable effective amount of ZnO mixed with BITS with the formation of a complex of the immobilized BIT/ZnO. Immovable effective amount of ZnO is an amount, effective for immobilization of antimicrobial agent of BITS in the complex of the immobilized BIT/ZnO. Found that excess immovable agent more effectively immobilized antimicrobial agent. An appropriate number of immovable agent may depend on a number of factors, including the nature of the substrate to be protected, and the conditions and length of time in which this substrate is used. An appropriate number of immovable agent for a particular purpose can be determined by routine testing immobilization of antimicrobial agent varying amounts of added immovable agent. Methods of assessment lack of mobility antimicrobial agent such as HPLC, known and available to specialists in the art and described in the examples section of this specification. Thus, depending on such factors as the ratio of the masses/mass BIT of ZnO can be in very wide limits. Typically, the ratio of the masses/mass BITS:ZnO should be from about 1:20 to about 3:1. Preferably the ratio of the masses/mass BITS:ZnO should be from about 1:10 to about 3:1, more preferably from about 1:5 to about 1:1 and most preferably from about 1:3 to about 2:3.

For the purposes of this invention "immobilized BIT" and "free BITS" are defined in business terms on the basis of the fact that the BIT itself is soluble in methanol at a concentration higher than 5%, i.e. 5 grams of pure BITS should be completely dissolved in 100 ml of methanol. When a solid complex of the BIT/ZnO obtained in accordance with this invention, shaken at ambient temperature (room) with the amount of methanol which constitute its twenty(20) times the mass, any BIT that goes into the solution, i.e. does not remain attached to ZnO, defined as "free" or "immobilized" BIT while the BIT that remains attached to ZnO as part of the solid, undissolved complex BIT/ZnO, defined as "immobilized BIT." Accordingly, the difference between the total to what iCustom BIT in the complex BIT/ZnO and the number of "free" BITS (i.e. the number of BITS, soluble in a predetermined amount of methanol) is the number of immobilized BIT" in the complex BIT/ZnO.

Analytical HPLC methods described in the examples section of this specification, offer a convenient way to analyze complex BIT/ZnO, to determine how many BITS it is "free", and how many BITS it is "immobilized". (For example, if a sample of 500 mg of the complex of the BIT/ZnO, which was approximately 33% mass/mass BIT, shaken with 100 ml of methanol, the sample must contain less than 170 mg of BITS, and if the whole BIT is free, it should all be dissolved in methanol, forming less than 0.2% solution.) Since the solubility of BITS in methanol at ambient temperature is more than 5%, this analysis clearly illustrates any immobilization BIT so that any number of BITS, which is not soluble in methanol, obviously immobilized in the complex BIT/ZnO.

Generally, it is desirable to maximize the number of BITS is "immobilized BIT" in the complex BIT/ZnO, and to minimize the amount of "free BITS" for the purposes of this invention, it is clear that in particular circumstances it may be preferable to have a mixture that is opposite to maximize "immobilized BIT complex. Complex ZnO/is it where from about 40% to about 100% of the immobilized BIT shall be suitable for many applications where preferably from about 50% to about 100%, more preferably from about 70% to about 100% and most preferably from about 90% to about 100%.

Typically, the complex is immobilized BIT/ZnO obtained by deposition in a dispersion concentrate when the particle size that is small enough to use directly in the coating material. The desired particle size of the complex BIT/ZnO may depend on a number of factors, including the nature of the substrate to be protected, and the conditions and length of time in which this substrate is used. The particle size of the complex BIT/ZnO can be adjusted by grinding, as, for example, a bead mill, and it can be in the range from nanoscale (about 10 nm) to several hundred microns. The particle size of the complex BIT/ZnO may be in the range from 0.8 μm to 50%/10 μm 95%. Preferably the particle size of the complex BIT/ZnO may be in the range from 1 μm to 50%/8 μm 95%, more preferably from 1.5 μm to 50%/6 microns 95%, and most preferably from 2.5 μm to 50%/4 microns 95%.

The viscosity of the dispersion concentrate complex BIT/ZnO can be adjusted to directly use it in the coating material. The viscosity of the complex BIT/ZnO may depend the et from a number of factors, including the nature of the coating and substrate to be protected. The viscosity of the complex BIT/ZnO can be adjusted to meet specific application of the final product. The viscosity of the dispersion concentrate complex BIT/ZnO can be adjusted by adding an agent regulating the viscosity. The preferred agent regulating the viscosity is xanthan gum (Kelzan®). The viscosity of the dispersion concentrate complex BIT/ZnO may be in the range from about 400 to about 1200 mPas, preferably from about 400 to about 1100 mPas, more preferably from about 400 to about 1000 mPas and most preferably from about 400 to about 900 mPas.

In accordance with the invention, the antimicrobial complex of the immobilized BIT/ZnO can be included in the final formulation for use in such end products as paints, coatings, plastics, wood products, wood composites, wood plastic composites, injection molding plastics, construction materials, paper, compositions based on starch, adhesives, plaster, concrete, sealants, gaskets, fabric, and rope products, textiles and the like, in a wide range of active concentrations of from about 0,004% to 2.0%. Such compositions can be prepared from the components of the investments of high concentrations of immobilized complex by appropriate dilution. Optimal utility interval is approximately from 0.01% to 1.0% of the immobilized complex in the final preparations for such systems the final application. When using such a modified product in the end application it is possible to protect the substrate for extended periods of time against the growth of microorganisms.

Compositions of the present invention, as a rule, should be prepared by mixing or dispersing the immobilized complex in the selected ratio with the liquid medium for dissolution or suspension of the active components. This medium may contain a diluent, emulsifier and wetting agent. The expected antimicrobial immobilized in the complex include the protection of paints and coatings, water-based adhesives, adhesives for welds, gaskets, mastics, inks, media for metal processing (process oils), polymer emulsions, dispersions of pigments, water industrial products, lubricants, sealants and the like. Antimicrobial immobilized complex can be represented in the form of liquid mixtures, in the form of irrigated powders, dispersions or in any other suitable form of product that is desired. In this regard, the composition of the present invention can be represented in the form the of the product, ready to use, in the form of aqueous dispersions, oily dispersions or in the form of a concentrate.

Useful solvents that can be used to obtain products containing antimicrobial immobilized complex, are some glycol ethers and esters, such as propylene glycol n-butyl ether, propylene glycol tert-butyl ether, 2-(2-methoxymethylethoxy)-tripropyleneglycol methyl ether, propylene glycol methyl ether, dipropyleneglycol methyl ether, tripropyleneglycol methyl ester and esters of the aforementioned compounds. Other useful solvents are n-organic n-pencilpoint and dibasic esters of some dicarboxylic acids, and mixtures thereof. Preferred solvents for these products are propylene glycol n-butyl ether, 1-methoxy-2-propanol and dibasic isobutyl ether mixture of succinic, glutaric and adipic acids.

For the production of preparations according to the present invention for specific applications composition also should probably provide adjuvants, common used in compositions intended for such applications, such as organic binders, additional antimicrobial agents, auxiliary solvents, processing additives, isatori, plasticizers, UV-stabilizers and / or amplifiers stability, water-soluble or water-insoluble dyes, colored pigments, siccatives, corrosion inhibitors, anti-settling, anti formation of surface crusts and the like.

Immobilization BIT on ZnO can be further controlled by adding to the set of basic salts of carboxylic acids such as fatty acids. Preferred fatty acids are benzoic acid, octanoic acid, 2-ethylhexanoate acid, novanova acid, cekanova acid, undecanoate acid, stearic acid, oleic acid and mixtures thereof.

In accordance with the present invention, the substrates to protect against contamination by microorganisms simply by treating the substrate with a composition containing an antimicrobial complex of the immobilized BIT/ZnO according to the present invention. Such processing may include mixing the composition with the substrate, coating, or otherwise bringing into contact of the substrate with the composition, and the like.

The following examples are provided for illustration and explanation of the invention. Unless otherwise noted, all references to share and percentages here and throughout the claims are based on weight.

EXAMPLES

Analytical method of determining the amount of immobilized BIT in the complex BIT/ZnO

D. the config analysis allows to determine the total number of BITS and the number of "free" BIT in the complex BIT/ZnO. The difference between the total number of BITS in the complex BIT/ZnO and the number of "free" BITS (i.e. the number of BITS soluble in a predetermined amount of methanol) is defined as the number of immobilized BIT" in the complex BIT/ZnO.

1. Analysis of the total number of BITS in the complex BIT/ZnO

To analyze the total number of BITS in the complex BIT/ZnO complex BIT/ZnO should be subjected to hydrolysis to release the BIT so that it can be analyzed using standard HPLC methods.

Hydrolysis

About 200 mg of a complex of the immobilized BIT/ZnO accurately weighed (exact weight may vary depending on the expected total number of BITS in the analyzed complex) in a 100 ml flask. Then add 20 ml of methanol (HPLC grade) and 5 ml of hydrochloric acid (1 mol/l). The flask is heated to approximately 50°C for 15 minutes. After cooling to ambient temperature the flask with methanol up to 100 ml mark and Then the reaction mixture was filtered through a membrane filter of 0.25 μm (e.g., Millipore), and it is ready for injection on the HPLC column.

Conditions of HPLC

DeviceThe apparatus Shimadzu A6
Column:Nucleosil 10-5 C18 HD (Macherey-Nagel)
The current gradient solvent:1.3 ml/min
Wavelength UV detector:312 nm
Eluent A:water +5% acetonitrile (:about)
Eluent:acetonitrile

The current time (min)Gradient solvent*
0,110% Eluent B + 90% Eluent And
3,010% Eluent B + 90% Eluent And
8,070% Eluent B + 30% Eluent And
10,070% Eluent B + 30% Eluent And
11,090% Eluent B + 10% Eluent And
to 12.090% Eluent B + 10% Eluent And
13,010% Eluent B + 90% Eluent And
15,010% Eluent B + 90% Eluent And
of 17.0stop
*=about:

Then sum the ary number of BITS in the complex BIT/ZnO determined by comparison with an external standard (150 mg-BIT/1 liter of methanol).

2. The analysis of the "free" BIT

BIT is highly soluble in methanol and can be extracted from the complex BIT/ZnO to determine the number of "free" BIT.

About 500 mg of the complex of the BIT/ZnO accurately weighed (exact weight may vary depending on the expected content of the "free" BIT of the analyzed complex) in a 100 ml flask. Add 50 ml of methanol (HPLC grade). Then the flask containing the mixture, voiced by ultrasound in a water bath for about 15 minutes. After cooling to ambient temperature the flask with methanol up to 100 ml mark and Then the reaction mixture was filtered through a membrane filter of 0.25 μm (e.g., Millipore), and it is ready for injection on the HPLC column.

The HPLC conditions for analysis of "free" BITS are the same as outlined above in part 1. Then the number of "free" BIT in the complex BIT/ZnO determined by comparison with an external standard (150 mg-BIT/1 liter of methanol).

Example 1

Comparative example bis-(1,2-Benzisothiazolin-3-one)zinc(II)chloride

Bis-(1,2-benzisothiazolin-3-one)zinc(II)chloride was obtained in accordance with example 53 U.S. patent No. 4150026.

1.5 g of 1,2-benzisothiazolin-3-one (analytical purity) was dissolved in 75 ml of absolute methanol. Added the number of 0.68 g of zinc chloride to obtain a clear solution is. The solvent is then evaporated in vacuo, and the residue was dried. Received a number of 2.1 g of bis-(1,2-benzisothiazolin-3-one)zinc(II)chloride. The molar ratio of BITS:Zn=2:1.

1,2-Benzisothiazolin-3-he was not immobilized in the form of a salt complex of bis-(1,2-benzisothiazolin-3-one)zinc(II)chloride, since this complex is almost completely soluble in methanol. The HPLC analysis showed that 63% of this salt complex was 1.2-benzisothiazolin-3-one, obtained from the methanol extract.

Example 2

The dispersion concentrate BIT/ZnO from BIT - potassium salt

The amount of 300 g of tap water was mixed with 26.7 g of prilled potassium hydroxide and to 74.1 g of commercially available 1,2-benzisothiazolin-3-one (90%) (available from Aldrich company) to produce a clear solution. Then add the amount of 270 g of water, 40 g of Emulsogen TS 200 (dispersing agent available from the company Clariant), 40 g of Atlox®4913 (non-ionic dispersing agent available from Unigema), 155,7 g of zinc oxide (available from Aldrich) and 30.1 g of zinc chloride (available from Aldrich), and the party was ground in a bead mill. The foam was adjusted by adding 0.5 g Rhodorsil 416 (inhibitor pricing based on silicone, available from Rhodia). The pH value was 7. The mixture was passed 3 times through a bead mill to reduce particle size. The product is made of dovecote 420 mPas (Spindle 4, Brookfield) adding and dispersing 4 g of xanthan gum (Kelzan®) and 59 g of water. The ratio of the masses/mass ZnO:BIT=of 2.6:1, and the molar ratio of BITS:Zn=0,20.

Received 1000 g (1,2-benzisothiazolin-3-one)of zinc oxide. The distribution of particle size: 1.3 micrometer 50%/5.5 micrometer 95%. Analysis: 6.7% of total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decomposition in 10% hydrochloric acid, neutralization, dilution with methanol, HPLC analysis of the BIT). Analysis of soluble BIT of a methanol extract: 2.4 percent. (64% of the total BITS is fixed on the surface of ZnO).

Example 3

The dispersion concentrate BIT/ZnO from BHT-ZnCl2

The amount of 90 g of tap water were mixed from 22.2 g of commercially available 1,2-benzisothiazolin-3-one (90%), 12 g of Emulsogen TS 200, 12 rAtlox®4913, to 46.7 g of zinc oxide and 9.0 g of zinc chloride. The batch was neutralized to pH 8.5 by slow addition with stirring of 16 g of 50% (mass/mass) solution of potassium hydroxide. The mixture was passed 3 times through a bead mill to reduce particle size. The foam was adjusted by adding 0.5 g Rhodorsil 416. The product is then brought up to a viscosity of 720 mPas (Spindle 3, Brookfield, 100 rpm) by adding and dispersing 1.6 g xanthan gum and 121 g of tap water. The ratio of the masses/mass ZnO:BIT=of 2.6:1, and the molar ratio of BITS:Zn=0,20.

Received a number of 400 g of the dispersion con is entrata (1,2-benzisothiazolin-3-one)of zinc oxide. The distribution of particle size: 0.8 micrometer 50%/3.5 micrometer 95%. Analysis: 6.7% of total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decomposition in 10% hydrochloric acid, neutralization, dilution with methanol, HPLC analysis of the BIT). Analysis of soluble BIT of a methanol extract is 1.1%. (84% of the total BITS is fixed on the surface of ZnO).

Example 4

The dispersion concentrate of the BIT/ZnO from BIT-ZnCl2

The amount of 90 g of tap water were mixed from 22.2 g of commercially available 1,2-benzisothiazolin-3-one (90%), 12 g of Emulsogen TS 200, 12 rAtlox®4913, 20.6 g of zinc oxide and 9.0 g of zinc chloride. The batch was neutralized to pH 8.5 by mixing 16 g of 50% (mass/mass) solution of potassium hydroxide. The party was passed 3 times through a bead mill to reduce particle size. The foam was adjusted by adding 0.2 g Rhodorsil 416. The product is then brought up to a viscosity of 950 mPas (Spindle 3, Brookfield, 100 rpm) by adding and dispersing 1.8 g xanthan gum and 147 g of water. The ratio of the masses/mass ZnO:BIT=1,6:1, and the molar ratio of BITS:Zn=0,35)

Received a number of 400 g of the dispersion concentrate (1,2-benzisothiazolin-3-one)zinc oxide. The distribution of particle size: 1.3 micrometer 50%/6.0 micrometers 95%. Analysis: 6.7% of total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decay of 10% hydrochloric acid is you, neutralization, dilution with methanol, HPLC analysis BIT). Analysis of soluble BIT of a methanol extract: of 1.6%. (76% of the total BITS is fixed on the surface of ZnO).

Example 5

The dispersion concentrate BIT/ZnO by direct deposition in a bead mill

The number to 166.2 g of tap water was mixed with 33.3 g of commercially available 1,2-benzisothiazolin-3-one (90%), 3 g of Emulsogen TS 200, 6 g of Atlox®4913 and 70.1 g of zinc oxide. The party was ground in a bead mill for 30 minutes. The foam was regulated by adding 0.3 g Rhodorsil 416. The product is then conveyed to the viscosity 1180 mPas (Spindle 3, Brookfield, 100 rpm) by adding 0.6 g of xanthan gum and 21 g of water. The ratio of the masses/mass ZnO:BIT=2,3:1, and the molar ratio of BITS:Zn=0,24.

Received an amount of 300 g of the dispersion concentrate (1,2-benzisothiazolin-3-one)zinc oxide. The distribution of particle size: 2.4 micrometer 50%/10 micrometers 95%. Analysis; 9.9% of total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decay of 10% hydrochloric acid, neutralization, dilution with methanol, HPLC analysis BIT). Analysis of soluble BIT of a methanol extract: 2.8 per cent. (72% of the total BITS is fixed on the surface of ZnO).

Example 6

The dispersion concentrate BIT/ZnO by direct deposition in a bead mill

The product from Example 5 was ground for 4 hours. It was Paul who told the amount of 300 g of the dispersion concentrate (1,2-benzisothiazolin-3-one)zinc oxide.

The distribution of particle size: 1.0 micrometer 50%/ 4.5 micrometer 95%. Analysis: 9,8% of total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decay of 10% hydrochloric acid, neutralization, dilution with methanol, HPLC analysis BIT). Analysis of soluble BIT of a methanol extract: of 0.8%. (92% of the total BITS is fixed on the surface of ZnO).

Example 7

The dispersion concentrate BIT/ZnO by direct deposition in a bead mill

The amount of 140 g of tap water was mixed with 6.7 g of commercially available 1,2-benzisothiazolin-3-one (90%), 3 g of Emulsogen TS 200, 6 g of Atlox 4913 and 134 g of zinc oxide. The party was ground in a bead mill for 4 hours. The foam was adjusted by adding 0.1 g Rhodorsil 416. The product is then conveyed to the viscosity 1180 mPas (Spindle 3, Brookfield, 100 rpm) by adding 0.6 g of xanthan gum and 10 g of water. The ratio of the masses/mass ZnO:BIT=20:1, and the molar ratio of BITS:Zn=0,028.

Received an amount of 300 g of the dispersion concentrate (1,2-benzisothiazolin-3-one)zinc oxide. The distribution of particle size: 1.5 micrometer 50%/7.7 micrometer 95%. Analysis: 2,0% total 1,2-benzisothiazolin-3-one by HPLC after acid hydrolysis (hydrolytic decay of 10% hydrochloric acid, neutralization, dilution with methanol, HPLC analysis BIT). Analysis of soluble BIT of a methanol extract is 0.1%. (95% of the total BIT fixed owano on the surface of ZnO).

Example 8

Solid immobilized BIT/ZnO

The number of 30 g (198 mmol) of 1,2-benzisothiazolin-3-one and 15 g (110 mmol) of zinc chloride was heated to boiling with delegacia in 250 ml of methanol. The resulting clear solution was cooled to approximately 50°C and was added 70 g (860 mmol) of zinc oxide. Then this mixture was heated to boiling with delegacia for 1 hour under stirring, and then cooled to room temperature. The solid was filtered and washed with 250 ml portions of methanol until such time as the chloride could not be detected in the filtrate by testing with silver nitrate in sulfuric acid. The complex BIT/ZnO was dried in vacuum to constant weight to obtain 90 g of a white powder. The ratio of the masses/mass ZnO:BIT=2.57 m:1, and the molar ratio BHT:ZnO=0,20.

The product of the BIT/ZnO was analyzed by heating to 300 mg at 60°C for 10 minutes with 50 ml of 5% sodium hydroxide solution in methanol. Sufficient methanol was added to bring the solution to 100 ml, and the resulting solution was filtered through the 0.45 micron filter and injected on the HPLC column RP-18 (eluent was a mixture of acetonitrile/water). The number of BITS determined using an external standard and a UV detector operating at 310 nm. theoretical yield of 96% based on BITS was achieved for complex BIT/ZnO, which results tester the training was free of chloride. (96% of the total BITS is fixed on the surface of ZnO).

Example 9

The dispersion concentrate immobilized BIT/ZnO from BIT - potassium salt

The amount of 45 g of prilled potassium hydroxide, 125 g of 1,2-benzisothiazolin-3-one (80% BIT, Mergal®BIT technical, commercially available from the firm Troy GmbH) and 20 g of Emulsogen TS 200 mixed in 440 g of water to obtain a clear solution. 234 g of zinc oxide were mixed and added to 12.5 g of Emulsogen TS 200. The foam was adjusted by adding 0.5 g Rhodorsil 416. Then added 45 g of zinc chloride, and the temperature was raised to 40°C. the pH was brought to 8 by adding 30 g of hydrochloric acid (16%). The mixture was passed 3 times through a bead mill to reduce particle size. The product is brought up to a viscosity of 440 mPas (Spindle 4, Brookfield) by adding 2 g of xanthan gum. The ratio of the masses/mass ZnO:BIT=of 2.6:1, and the molar ratio of BITS:ZnO=0,20.

Received a quantity of 1000 g (1,2-benzisothiazolin-3-one)of zinc oxide.

The distribution of particle size: 19 micrometers 50%/79 micrometres 95%. Analysis: 10,0% 1,2-benzisothiazolin-3-one by HPLC after alkaline hydrolysis.

Example 10

The infrared spectrum of BITS

A sample of the BITS used for the analysis of the infrared spectrum in Fig.

1. was an analytical standard Mergal (99,56%) from Troy Corporation. The sample was obtained in accordance with standard techniques in the form of presova the Oh (10-20%) KBr(99%)pill, using the instrument Perkin-Elmer System 2000 FT-IR.

Example 11

The infrared spectrum of the ZnO ZnO Sample used for the analysis of the infrared spectrum in Fig.

2. were of analytical purity (99+%). The analysis of the infrared spectrum is the same as described in Example 10.

Example 12

The infrared spectrum of the complex BIT/ZnO

A sample of the BIT/ZnO used for the analysis of the infrared spectrum in figure 3, was a complex obtained in example 8. The analysis of the infrared spectrum is the same as described in Example 10.

Example 13

The infrared spectrum BITS/Li salt

Sample BIT/Li salts used for the analysis of the infrared spectrum in figure 4, consisted of a standard analytical purity (99%) of Mergal. The number of 202 g (1 mol) BIT (Proxel Press Paste, Arch) in the form of a 75% wet cake (residual water) and 45 g (1.07 mol) of hydrate of lithium hydroxide was heated to boiling with delegacia within one hour in 700 ml of methanol. Then the mixture was cooled to ambient temperature to precipitate BIT - lithium salt, which was isolated by filtration and dried to constant weight. The analysis of the infrared spectrum is the same as described in Example 10.

Example 14

The activity of a complex of the immobilized BIT/ZnO in the paint for Matt coatings on water basics is against Pseudomonas aeruginosa using a modified Swiss standard test SNV195120

The activity of a complex of the immobilized BIT/ZnO from example 8 as a dry film biocide against Pseudomonas aeruginosa DSM 939 was determined in the paint ICI UK, Diamond Matt, commercially available interior paint, matte water-based coatings (40% acrylic substances) in accordance with a modified Swiss standard test SNV195120, which is described below.

Preparation of test sample:

The complex of the immobilized BIT/ZnO from example 8 was included in interior paint matte coatings water based on the levels shown in the table below. The colors gave be balanced for one week at room temperature.

A quantity of 50 mg of the complex of the BIT/ZnO were mixed with 100 g of the ink is obtained by 0.05% sample 1 in the table below, other samples were obtained respectively). Round filter paper (diameter 5.5 cm) was covered with the test material to a thickness of 150 g/m2wet, and the resulting samples were dried at room temperature.

One half of the test specimen were washed with tap water (9 litres per m2) in a beaker. The samples were dried at room temperature and sterilized by gamma radiation from a source of cobalt 60 (25 kGy). In microbiological test Pseudomonas aeruginosa DSM 939 used in quality the be source of bacteria.

Liquid culture of each bacterial strain were incubated overnight at the appropriate temperature, and then diluted 1:100000 with results in account 104 CFU in ml. of 0.1 ml of these diluted cultures subcultured on bacterial nutrient medium in Petri dishes. The test samples were placed coated side down on the inoculated nutrient medium and incubated for 1 day at 29°C.

The growth of bacteria on the agar under the tested sample was evaluated as follows:

0N the Absence of bacterial growth under the sample, the zone of inhibition on a nutrient medium.

0 No bacterial growth under the sample.

G bacteria Growth under the sample.

Bacterial growth under the sample was observed under unprotected friendly material. Antibacterial protection was provided, if there were no bacteria growth under the sample.

No. of
times
CA
Designation sampleAntimicrobial active concentration %Weight of film (g/m2)Psa newima-
Tye
Psa washed after 24 hNotes
1Interior paint, matte coatings** + 0.05% of IMM is britannico BITS/sample 8 BIT*
0,016%
1820G
2Interior paint, matte coatings** + 0.1% of the immobilized BIT/sample 8BIT*
to 0.032%
21200
3Interior paint, matte coatings** + ThiramThiram 0,1%2230GComparative example
4Interior paint, matte coatings** + ThiramThiram 0,2%1950GComparative example
5Interior paint, matte coatings** + ZirThe Zir 0,1%2090GComparative example
6 Interior paint, matte coatings** + ZirThe Zir 0,2%1860HGComparative example
7Interior paint, matte coatings** - net controlno255GGThe growth control
*BIT = 1,2-benzisothiazolin-3-one, total concentration
** Interior paint, matte coatings = ICI UK, Diamond Matt
Thiram = tetramethylthiuram disulfide
The Zir = (T-4)-bis(dimethyldithiocarbamate-S,S')zinc)

In this test demonstrated the effectiveness of the complex immobilized BIT/ZnO from Example 8 at a very low concentration against Pseudomonas aeruginosa in interior paint, matte water-based coatings (40% acrylic material) using a modified Swiss standard test SNV195120. This effect was still present after artificial aging (24 hours of leaching, immersion in water), which demonstrates the long shelf life of antimicrobial substrate with immobilized 1,2-benzisothiazolin-3-one, compared with the OBR is scami paint with the common defense, missing after washout.

Example 15

The activity of a complex of the immobilized BIT/ZnO in semi-gloss water-based against Pseudomonas aeruginosa using a modified Swiss standard test SNV195120

The activity of a complex of the immobilized BIT/ZnO from example 8 as a dry film biocide against Pseudomonas aeruginosa DSM 939 was determined in a commercially available interior semi-gloss water-based (40% acrylic substances with activator bonding) in accordance with a modified Swiss standard SNV195120. The paint composition, which is usually applied in wet areas, outlined below. Microbiological test was performed in accordance with the procedure described in Example 14.

ComponentNumber
Water16 g
Hydroxymethylcellulose0.2 g
Calgon N0.1 g
Titanium dioxide (rutile)15 g
The magnesium aluminosilicate3 g
White porcelain clay5 g
Calcium carbonate Calcite12.5 g
Iron oxide3 g
Mowilith DM 772 (polyacrylate dispersion Celanese (formerly known as Clariant)40 g
Texanol4 g
Merral K14 (preservative for storage of a paint container)0.2 g
the pH was brought to 8.5 with ammonium hydroxide (25%)

no way-
CA
Designation sampleAntimicrobial active concentration %Weight of film (g/m2)Psa newima-
Tye
Psa washed after 24 hNotes
1Interior semi-gloss + 0,05% of the immobilized BIT/sample 8BIT*
0,016%
229G0Water-soluble paint ingredients that support growth, washed
2 Interior semi-gloss + 0.1% of the immobilized BIT/sample 8BIT*
to 0.032%
2310HE
3Interior semi-gloss + ThiramThiram 0,1%221GGComparative example
4Interior semi-gloss + ThiramThiram 0,2%222GGComparative example
5Interior semi-gloss - net controlno221GGThe growth control
*BIT = 1,2-benzisothiazolin-3-one total concentration
Thiram = tetramethylthiuram disulfide

In this test demonstrated the effectiveness of the complex immobilized BIT/ZnO from Primera at very low concentration against Pseudomonas aeruginosa interior semi-gloss water-based (40% acrylic substances with activator bonding) using a modified Swiss standard test SNV195120.

Example 16

The activity of a complex of the immobilized BIT/ZnO in the paint to dull water-based coatings against Escherichia coli using test JISZ2801:2000(E)

The activity of a complex of the immobilized BIT/ZnO from example 9 as a dry film biocide against Escherichia coli was determined in the paint ICI UK, Diamond Matt, commercially available interior paint, matte water-based coatings (40% acrylic substances) in accordance with the test JIS Z2801:2000 (E) (Japanese industrial standard test Z2801:2000 (E), Antimicrobial products - Test for antimicrobial activity and efficacy).

The complex was applied on the control panel Leneta Scrub Resistance when the thickness of the dry film 200 micrometers foam roller, giving time for 18 hours drying between coats. The panel was balanced in the dark for 7 days. Cut out the secondary samples (each 50 mm × 50 mm). Samples were inoculable suspension of test bacteria, and then incubated in chambers (1) at 20°C and 65%relative humidity.

For selection of bacteria used scrapings. From a sample of pure control was allocated to 1.8×105CFU/cm2. This number was taken as the initial bacterial load on the surface.

In this test demonstrated the effectiveness of the complex immobilized B Is T/ZnO from Example 9 at a very low concentration against Escherichia coli in interior paint, semi-gloss coatings, water-based (40% acrylic substances) using test JIS Z2801:2000 (E). Data show that Escherichia coli can survive for 8 hours on interior paint, semi-gloss coatings, water-based (40% acrylic substances), has not been processed by a complex of the immobilized BIT/ZnO. The complex of the immobilized BIT/ZnO reduced the level of bacteria 99.8%, whereas the commercially available comparative material level of decline was much lower.

Example 17

The activity of a complex of the immobilized BIT/ZnO in the paint to dull water-based coatings against Pseudomonas aeruginosa using test JIS Z2801:2000 (E)

No. of
times
CA
Designation sampleAntimicrobial active concentration %The time code is
the h
Log (CFU/cm2)The degree of inhibition, % relative to pure controlNotes
1AInterior paint - net controlnet control05,11-Dedicated inoculum
1BInterior paint - the number of the first control net control84,690%Control
2Interior paint + 0.15% of the immobilized BIT/sample 8BIT*
0,05%
8of 3.5692,70%
3Interior paint + 0,05% ZPTZPT
0,05%
84,1869,40%Comparative example
4Interior paint 2.5% of the variance IPBCIPBC
1,0%
84,5330,60%Comparative example

The activity of a complex of the immobilized BIT/ZnO from example 8 as a dry film biocide against Pseudomonas aeruginosa DSM 939 was determined in the paint ICI UK, Diamond Matt, commercially available interior paint, matte water-based coatings (40% acrylic substances) in accordance with the test JIS Z2801:2000 (E). Microbiological test was performed in the CE is accordance with the methodology described in Example 16.

ZPT = pyrithione zinc

IPBC = variance: 40% suspension concentrate 3-adpropinquaverant

*BIT = 1,2-benzisothiazolin-3-one total concentration

In this test demonstrated the effectiveness of the immobilized complex of the BIT/ZnO from Example 8 at a very low concentration against Pseudomonas aeruginosa DSM 939 in interior paint, semi-gloss coatings, water-based (40% acrylic substances) using test JIS Z2801:2000 (E).

Example 18

The activity of a complex of the immobilized BIT/ZnO in the paint to dull water-based coatings against Pseudomonas aeruginosa using test JIS Z2801

The activity of a complex of the immobilized BIT/ZnO from example 8 as a dry film biocide against Pseudomonas aeruginosa DSM 939 was determined in the paint described in example 15, in accordance with the test JIS Z2801. Microbiological test was performed in accordance with the procedure described in Example 16.

No. of
times
CA
Designation sampleProteomika-
Naya active concentration %
The contact time, hLog (CFU/cm2)The degree of inhibition, % relative to pure control Notes
1AInterior paint for walls - net controlnet control04,18Dedicated inoculum
1BInterior paint for walls - net controlnet control84,690%control
2Interior paint for walls + 0.15% of the immobilized BIT/sample 8BIT*
0,05%
81,08of 99.98%
3Interior paint for walls + 0,05% ZPTZPT
0,05%
8of 4.6639,5%Comparative example
4Interior paint for walls is 2.5% of the variance IPBCIPBC 0,1%84,34 71,1%Comparative example
ZPT = pyrithione zinc
IPBC = variance: 40% suspension concentrate 3-adpropinquaverant
*BIT = 1,2-benzisothiazolin-3-one total concentration

In this test demonstrated the effectiveness of the complex immobilized BIT/ZnO from Example 8 at a very low concentration against Pseudomonas aeruginosa in interior acrylic paint for the walls using JIS Z2801.

Example 19

The activity of a complex of the immobilized BIT/ZnO in the paint to dull water-based coatings against Pseudomonas aeruginosa using test JIS Z2801

Imitation severe environmental conditions

The activity of a complex of the immobilized BIT/ZnO from example 8 as a dry film biocide against Pseudomonas aeruginosa DSM 939 was determined in the paint described in example 15, in accordance with the test JIS Z2801. Microbiological test was performed in accordance with the procedure described in Example 16. After equilibration, the samples were washed in water (24 hours) to simulate the conditions of use in severe environmental conditions. The paint film was cleaned with a water jet.

No. of
times
CA
Designation sampleProteomika the th active concentration, %The contact time, hLog (CFU/cm2)The degree of inhibition, % relative to pure controlNotes
1AInterior paint for walls - net controlnet control04,18Dedicated inoculum
1BInterior paint for walls - net controlnet control243,880%control
2Interior paint for walls + 0.15% of the immobilized BIT/sample 8BIT*
0,05%
242,5295,7%
3Interior paint for walls + 0,05% ZPTZPT
0,05%
243.04 from85,5%Comparative
tion ol the measures
4Interior paint for walls is 2.5% of the variance RVSRVS
0,1%
243,7625,0%Comparative
hydrated sample
ZPT = pyrithione zinc
IPBC = variance: 40% suspension concentrate 3-adpropinquaverant
*BIT = 1,2-benzisothiazolin-3-one total concentration

In this test demonstrated the effectiveness of the complex immobilized BIT/ZnO from Example 8 at a very low concentration against Pseudomonas aeruginosa in interior acrylic paint for the walls using test JIS Z2801, simulating severe environmental conditions.

Example 20 the Activity of a complex of the immobilized BIT/ZnO in the paint to dull water-based coatings against Escherichia coli using a test

JIS Z2801

Imitation severe environmental conditions

The activity of a complex of the immobilized BIT/ZnO from Example 8 as a dry film biocide after artificial aging against Escherichia coli was determined in the paint ICI UK, Diamond Matt, commercially available interior paint, semi-gloss coatings, water-based (40% acrylic substances), in accordance with the test JIS Z2801. The paint samples were prepared, as is written in Example 19. Microbiological test was performed in accordance with the procedure described in Example 16. After equilibration, the samples were washed in water (24 hours) to simulate the conditions of use in severe environmental conditions. The paint film was cleaned with a water jet.

No. of
times
CA
Designation sampleAntimicrobial active concentration %The time code is
the h
Log (CFU/
cm2)
The degree of inhibition, % relative to pure controlNotes
1AInterior paint for walls - net controlnet control03.04 fromDedicated inoculum
1BInterior paint for walls - net controlnet control243,300%Control
2Interior paint for walls and furniture is + 0.15% of the immobilized BIT/sample 8 BIT*
0,05%
242,7373%
3Interior paint for walls + 0,05% ZPTZPT
0,05%
243.04 from20%Comparative example
4Interior paint for walls is 2.5% of the variance IPBCIPBC
0,1%
243,7635%Comparative example
ZPT = pyrithione zinc
IPBC = variance: 40% suspension concentrate 3-adpropinquaverant
*BIT = 1,2-benzisothiazolin-3-one total concentration

In this test demonstrated the effectiveness of the complex immobilized BIT/ZnO from Example 8 at a very low concentration against Escherichia coli in interior paint, matte water-based coatings (40% acrylic substances) using test JIS Z2801, simulating severe environmental conditions.

Example 21

Leaching of a complex of the immobilized BIT/ZnO in the paint VOC water-based

The paint on in the basis with a low content of volatile organic compounds (VOC) were prepared in accordance with the following formula:

Filler
Ingredient:% mass/masscomments
Watera 21.75
Walocel HM 30,000 PV0,20EUMM modified
Calgon N new0,20polyphosphate
Sodium hydroxide 25%0,10the pH regulator
Borchigel 760,25%
Borchigen NA400,50%
Kronos 216010,00%Pigment rutile
Finntalc M 30 SLto 5.00%Filler
White porcelain clay4,00%Filler
Omyacarb 10GU19,60%Filler
Omyacarb 5 GU10,00%
Milled basis for 30 min at 2000 cycles/min
Mowilith LDM 187123,00%Binder copolymer and ethylene vinyl
Waterof 5.40%

Preparation of test sample:

The complex is immobilized BIT from example 9 (10% BITS) included as the last component in the paint at the levels indicated in the table below. As a comparative compound in the paint consisted of a commercially available solution of BIT-lithium (Mergal® K10N) (samples 2 and 4) in the same way. The test paints were made to be balanced out in one week at room temperature. Round filter paper (diameter 5.5 cm) was covered with the tested paints, and the resulting samples were dried at room temperature. The tested samples were washed with tap water (9 litres per m2) in a beaker. After the time periods specified in the table below, the test samples were taken and dried at room temperature. The total concentration of the BITS in the test paint films were analyzed by HPLC after selecing the hydrolysis and extraction of the washed films of paint.

Education
set of technical documents No.
An antimicrobial agent added to the paintAntimicrobial active substance BITS, % mass/mass to wet mass of colors8 h washout, % BIT*24 h washout, % BIT*Comments
10.3% of the immobilized BIT example 90,03%4217
2a 0.3% aqueous solution of 10% lithium BIT of salt0,03%21Comparative example
30.5% of the immobilized BIT example 90,05%4924
4a 0.5% aqueous solution of 10% lithium BIT of salt0,05%11Comparative example

The results of expr which are in the form % found the number from the original ("unwashed") sample of the paint. This eliminates the error in the result of differences in the method of extraction and the degree of selection.

This example illustrates the immobilization of the complex BIT/ZnO in the film paints VOC water-based.

Example 22

Leaching of a complex of the immobilized BIT/ZnO in alkyd-acrylic paint

The test paint was a commercially available paint Larco type 147 (Denmark), water soluble outer coating for wood surfaces based on alkyd-acrylic binder mixture. The complex is immobilized BIT from example 9 included in this paint, and test samples of the paint film was prepared as described in example 21. After equilibration, the samples of paint were washed as described in example 21. Wash water was changed after 24 hours.

Education
set of technical documents No.
An antimicrobial agent added to the paintAntimicrobial active substance BITS, % mass/mass to wet mass of colors8 h washout, % BIT*24 h washout, % BIT*Comments
10.3% of the immobilized BIT example 90,03%5027
2a 0.3% aqueous solution of 10% lithium BIT of salt0,03%70Comparative example
30.5% of the immobilized BIT example 90,05%4736
4a 0.5% aqueous solution of 10% lithium BIT of salt0,05%102Comparative example

This example illustrates the immobilization of the complex BIT/ZnO in a commercially available water-based paint for exterior coatings for wood surfaces based on alkyd-acrylic binder mixture.

Although the invention is illustrated with reference to specific and preferred embodiments, specialists in the art should be understood that variations and modifications can be made by routine experimentation and practice of the invention. Thus, the invention is not intended to limit the description above, but should be defined by the attached fo what moloi of the invention and its equivalents.

1. The method of producing complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide, including
(a) heating 1,2-benzisothiazolin-3-one and zinc chloride to a boil with delegacia in C1-C4branched or unbranched alcohol with formation of a solution,
(b) cooling of this solution and add immovable effective amount of zinc oxide to the solution with the formation of the mixture,
(C) heating the mixture to a boil with delegacia, and then cooling the mixture to room temperature,
(g) filtering the mixture to obtain complex immobilized 1,2-benzisothiazolin-3-one/zinc oxide.

2. The method according to claim 1, where the ratio of wt./wt. 1,2-benzisothiazolin-3-one:zinc oxide is from about 1:20 to about 3:1.

3. The method according to claim 1, where the besieged complex includes at least about 40% immobilized 1,2-benzisothiazolin-3-it is based on the 1,2-benzisothiazolin-3-it is used to prepare the complex.

4. Antimicrobial composition which is suitable for providing antimicrobial activity to the surface of a solid substance containing 1,2-benzisothiazolin-3-one or its salt, which is immobilized in the form of the complex 1,2-benzisothiazolin-3-one/zinc oxide obtained by the method according to claim 1.

5. The composition according to claim 4, where the ratio of wt./wt. 1,2-benzisothiazolin-3-one:the zinc oxide with the hat from about 1:20 to about 3:1.

6. The composition according to claim 4, where the immobilized 1,2-benzisothiazolin-3-one/zinc oxide has a distribution of particle size is from about 0.8 μm to 50%/3.5 µm 95% to about 19 μm 50%/79 μm 95%.

7. The composition according to claim 4, containing an additional component from the group consisting of antimicrobial agents and antifungal film preservatives.

8. The composition according to claim 7, where the additional component is selected from methylbenzimidazole-2-ylcarbamate, 3-iodine-2-propynylbutylcarbamate, pyrithione zinc, 5-chloro-2-(2,4-dichlorophenoxy)phenol, 2-n-acterization-3-one, 4,5-dichloro-2-n-acterization-3-one, 2,4,5,6-tetrachloroisophthalonitrile, 3-benzo[b]Tien-2-yl-5,6-dihydro-1,4,2-oxathiazine 4-oxide, zinc bis(dimethyldithiocarbamate), tetramethylthiuram disulfide, 2-n-butylbenzothiazole-3-one, silver and silver compounds, compounds zinc silver zeolite, silver chloride on titanium dioxide and silver nanoparticles.

9. The composition according to claim 4, further containing adjuvants selected from the group consisting of organic binding agents, auxiliary solvents, additives, retainers, plasticizers, UV-stabilizers or amplifiers stability, water-soluble or water-insoluble dyes, color pigments, siccatives, corrosion inhibitors, anti-settling, anti-superficial education is th cover basic and complex salts of carboxylic acids.

10. The composition according to claim 4, where the composition shows an infrared spectrum, which does not include the band at 1645 cm-1.

11. The use of a composition according to any one of claims 4 to 10 as an antimicrobial agent.

12. The application of claim 11, where the composition is used for the protection of paints and coatings, water-based adhesives, adhesives for welds, gaskets, mastics, inks, media for metal, polymer emulsions, pigment dispersions, aqueous industrial products, lubricants or sealants.



 

Same patents:

FIELD: chemistry.

SUBSTANCE: invention relates to fungus control, specifically to 5-iodotetrazole derivatives , in which R1 denotes butylene, straight unsubstituted alkyl with 8-16 carbon atoms, straight or branched unsubstituted or mono- or multi-, identically or differently substituted alkyl with 1-8 carbon atoms, where the substitutes are or mono- or multi-, identically or differently substituted alkyl residues selected from a group comprising unsubstituted alkoxy or 1-6 carbon atoms and alkoxy with 1-6 carbon atoms, substituted with dioxalonyl, phenyl which is up to five times identically or differently substituted with halogen, alkyl with 1-4 carbon atoms, halogenalkyl with 1-4 carbon aotms, alkoxy with 1-3 carbon atoms, alkylthio with 1-4 carbon atoms, morpholinyl, except the following compounds: 1-tert-butyl-5-iodotetrazole, 1-ethyl-5-iodotetrazole, 1-methyl-5-iodotetrazole. Said 5-iodotetrazole derivatives are obtained by treating tetrazoles of general formula , in which R1 assumes values given above, with iodine in an organic solvent in the presence of a base and, if needed, in the presence of a diluent. The invention also relates to a fungicidal agent, containing 5-iodotetrazole derivatives of general formula , in which R1 denotes hydrogen, alkylene with 1-4 carbon atoms, straight unsubstituted alkyl with 8-16 carbon atoms, straight or branched unsubstituted or mono- or multi-, identically or differently substituted alkyl with 1-8 carbon atoms, where the substitutes are mono- or multi-, identically or differently substituted alkyl residues selected from a group comprising unsubstituted alkoxy with 1-6 carbon atoms and alkoxy with 1-6 carbon atoms, substituted dioxalonyl, unsubstituted phenyl, phenyl which is up to five times identically or differently substituted with halogen, alkyl with 1-4 carbon atoms, halogenalkyl with 1-4 carbon atoms, alkoxy with 1-3 carbon atoms, alkylthio with 1-4 carbon atoms, morpholinyl and at least one solvent or diluent, as well as auxiliary additives if necessary. The invention also relates to paint material containing compounds of formula (Ia).

EFFECT: said fungicidal agent can be used in a method of protecting plants and paint materials from attack and/or decomposition by fungi by exposing the fungi or habitat thereof to the said agent.

11 cl, 2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to azole derivatives of formula I , where: A denotes S, O; W denotes -(C=O)-; X are identical or different and denote =C(-R)- or =N-; Y denotes -O- or -NR1-; R denotes hydrogen, halogen, (C1-C6)-alkyl, nitro; R1 denotes hydrogen; R2 denotes (C5-C16)-alkyl, (C1-C4)alkyl-phenyl, where phenyl can be optionally mono- or poly-substituted with (C1-C6)-alkyl; R3 denotes hydrogen; or R2 and R3 together with the nitrogen atom bearing them can form a monocyclic saturated 6-member ring system, where separate members of this ring system can be substituted with 1 group selected from the following: -CHR5-, -NR5-; R5 denotes (C1-C6)-alkyl, trifluoromethyl; and physiologically acceptable salts thereof. The invention also pertains to methods of producing said compounds and a medicinal agent based on said compounds.

EFFECT: novel compounds and a medicinal agent based on said compounds are obtained, which can be used as hormone-sensitive lipase (HSL) or endothelial lipase (EL) inhibitors.

12 cl, 11 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to novel compounds, which possess qualities to estrogen modulators, of general formula (1) or its pharmaceutically acceptable salt, where R1 represents hydrogen atom or (C1-C6)alkyl, -SO2NR7R8, phenyl (C1-C3)alkyl or (C1-C3)alkyl, substituted with 5-8-member heterocyclic radical, containing nitrogen atom; R2 and R3 each independently represents hydrogen atom or hydroxyl, halogen atom or (C1-C6)alkoxy; X represents O, S, SO, SO2 or NR4; R4 represents hydrogen atom or (C1-C6)alkyl, phenyl, phenyl(C1-C3)alkyl, (C1-C3)alkyl, substituted with 5-8-member saturated heterocyclic radical, containing one nitrogen atom, or group -COR7, -CO2R7 or -SO2NR7R8, where phenyl is not substituted or is substituted with at least one substituent, selected from group which includes hydroxyl, halogen atom or phenyl(C1-C3)alkoxy; Y represents direct bond, -(CR10R11)n- or -R10C=CR11-; R7 and R8 each independently represents hydrogen atom or (C1-C6)alkyl group; R10 and R11 each independently represent hydrogen atom or cyano, or group CONR7R8; n equals 1 or 2; A represents (C3-C12)cycloalkyl or phenyl, where phenyl is not substituted or is substituted with at least one substituent, selected from group which includes hydroxyl, halogen atom, (C1-C3)alkyl, (C1-C3)alkoxy; when X represents NR4, Y and R2 together with containing them indazole cycle can also form 1H-pyrano[4,3,2-cd)indazole; on condition that: 1) when X represents O, S or NR4, R1 represents hydrogen atom or (C1-C6)alkyl, and Y stands for direct bond, then A is not optionally substituted phenyl; 2) when X represents O, R1O represents 6-OH or 6-OCH3, Y represents direct bond and A represents cyclopeptyl, then (R2, R3) or (R3, R2) are different from (H, CI) in position 4, 5; 3) when X stands for O, R1O represents 6-OH, R2 and R3 represent H, and Y represents CH=CH, then A is not phenyl or methoxyphenyl; 4) when X represents SO2, A represents phenyl and R1O represents 5-or 6-OCH3, then (R2, R3) or (R3, R2) are different from (H, OCH3) in position 6- or 5-, compound not being one of the following: 3-phenyl-5-(phenylmethoxy)-1H-indazole; n-hydroxy-3-phenylmethyl-7-(n-propyl)-benz[4,5]isoxazole; 3-(4-chlorphenylmethyl)-6-hydroxy-7-(n-propyl)-benz[4,5]isoxazole; 6-hydroxy-3-(2-phenylethyl)-7(n-propyl)-benz[4,5]isoxazole; 3-cyclopropyl-6-hydroxy-3-phenylmethyl-7-(n-propyl)-benz[4,5|isoxazole; 3-cyclohexylmethyl-6-hydroxy-3-phenylmethyl-7-propyl-benz[4,5]isoxazole. Invention also relates to pharmaceutical composition, application and method of prevention and treatment of disease, where modulation of estrogen receptors is required.

EFFECT: obtaining novel compounds, which possess qualities of estrogen receptors modulators.

18 cl, 7 dwg, 8 tbl, 97 ex

FIELD: chemistry.

SUBSTANCE: invention relates to novel compounds of general formula

, where R1 is a

or or or group, R2 is morpholine or OR' or N(R")2; R' is a lower alkyl, a lower alkyl substituted with a halogen, or -(CH2)n-cycloalkyl; R" is a lower alkyl; R is NO2 or SO2R'; R4 is hydrogen, hydroxy, halogen, NO2, lower alkoxy, SO2R' or C(O)OR"; R5/R6/R7 denote hydrogen, halogen, lower alkyl; X'/X1 denote CH or N, provided that X1 /X1' are not CH at the same time; X2 is O or S; n equals 0 or 1, and to their pharmaceutically active acid-addition salts. The invention also relates to a drug.

EFFECT: obtaining novel biologically active compounds which are active as glycine transporter 1 inhibitors.

11 cl, 24 ex, 1 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to novel hexafluoroisopropanol-substituted ether derivatives of formula (I) to their pharmaceutically acceptable salts and to esters which are capable of bonding with LXR-alpha and/or LXR-beta, as well as to pharmaceutical compositions based on said compounds. In formula (I) R1 is hydrogen, lower alkyl or halogen, one of groups R2 and R3 is hydrogen, lower alkyl or halogen, and the second of groups R2 and R3 is -O-CHR4-(CH2)m-(CHR5)n-R6. Values of R4, R5, R6 m and n are given in the formula of invention.

EFFECT: novel compounds have useful biological properties.

22 cl, 4 dwg, 102 ex

The invention relates to new chemical compounds derived from anthra[2,1-d]isothiazol-3,6,11-trione General formula I, where a is the lowest alkylene, R1and R2(independent) - lower alkyl, or R1and R2together with the nitrogen atom form a six-membered saturated, a heterocycle, which may optionally contain a heteroatom such as oxygen atom, and their pharmaceutically acceptable salts

The invention relates to a method for producing 2-alkylbenzoates, which includes the interaction bisimide formula 2 in water or water-containing organic liquid bisulfite or allocating the bisulfite agent with the formation of salts of the Rebellion and the transformation of the salt Riot in alkaline conditions in the 2-alkyl-BIT
Disinfectant // 2490008

FIELD: medicine.

SUBSTANCE: disinfectant refers to veterinary medicine, particularly to disinfectants used for air sanitation and surface disinfection in livestock houses in the presence of animals, including poultry. The agent has an antiseptic effect, which allows using it in acute, chronic and sub-clinical mastitis, vaginitis, endometritis and other inflammatory processes of varying aetiology. An active ingredient is presented by a complex of dimethyl sulphoxide and crystalline iodine, succinic acid, fumaric and citric acids which provides better drug absorption and prolonged action. It is prepared in the form of mother liquor diluted in water immediately before use.

EFFECT: invention enables prolonging the shelf life when in use.

7 tbl

FIELD: chemistry.

SUBSTANCE: method of producing a disinfectant involves first carrying out polycondensation of hexamethylenediamine and guanidine hydrochloride. Polycondensation starts with preparation of a reaction mass in form of a suspension of crystalline guanidine hydrochloride in molten hexamethylenediamine, taken in ratio of 1:(1-1.5). The suspension is obtained by gradually adding crystalline guanidine hydrochloride, preheated to temperature of 90-120°C, to molten hexamethylenediamine and then stirring. The reaction mass is then heated in steps: holding for 4 hours at 120°C, then for 8 hours at 160°C and then for 3 hours at 180°C. Temperature is then gradually raised to 210°C at a rate of 3-4°C/h. The reaction mass is then subjected to vacuum treatment and cooled.

EFFECT: method enables to reduce toxicity of the end product and obtain a polymer with the required molecular weight and sufficient purity without washing steps.

2 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture and is meant for disinfecting vehicles and containers after transporting livestock cargo. The method involves treating vehicles and containers with a disinfectant. The disinfectant contains a solution of oxidants and additionally propylene glycol, sodium nitrite, sodium benzoate, products of reaction of glycerol with formic acid, with the following ratio of components, wt %: propylene glycol - 0.9-7.5, sodium nitrite - 0.27×10-3-16.5×10-3, sodium benzoate - 1.35×10-3-82.5×10-3, products of reaction of glycerol with formic acid - 0.18×10-3-11.0×10-3, solution of oxidants - the balance. The solution of oxidants is synthesised from 10.0-20.0% sodium chloride solution subjected to dc current with intensity which enables to achieve pH 7-8, concentration of active chlorine of 0.5-0.7% and redox potential of +1000±50 mV. Treatment is carried out once with consumption of the disinfectant of 0.15-0.25 l/m2 with exposure of 55-65 min; immediately after treating with the disinfectant, the surface of the vehicles and containers is further exposed for 30-60 min with constant UV radiation with wavelength of 254±5 nm with a dose of 12.8-25.6 J/cm2.

EFFECT: high efficiency of disinfecting vehicles and containers after transporting livestock cargo.

4 tbl, 3 ex

FIELD: medicine.

SUBSTANCE: invention relates to disinfectants. An antiseptic disinfectant contains the film-forming preparation iodopyrone containing 6-8% of active iodine and water, contains ethanol in the following proportions, wt %: iodopyrone - 1.0-1.3 (per active iodine basis), ethanol - 20, water - the rest. The antiseptic disinfectant represents a ready-to-use preparation presented in the form of a solution or a spray.

EFFECT: invention provides the qualitative and quantitative stability of the active substance in the easily water-washable disinfectant which does not stain and has a non-irritant, prolonged effect If kept in an unopened container, it has a shelf-life of 2 years from the date of manufacture.

3 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to bactericidal medication and can be applied for disinfection of livestock premises, placed in them technological equipment, implements for animal care, vehicles for transportation of animals, places where animals and other objects of veterinary supervision are concentrated. Medication includes alkyldimethylbenzylammonium chloride (ADMBAC), glutaric aldehyde, water and sodium hydroxide, taken in specified ratio. In case of specified ratio synergetic effect is observed and maximal bactericidal activity of medication, assessed by value of minimal bactericidal concentration (MBC), at which death of test-culture is observed, is reached.

EFFECT: invention ensures increase of bactericidal activity and reduction of medication toxicity with minimal content of active substances.

1 tbl, 15 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention relates to sanitation and can be applied in food, medical, veterinary, processing industry. Invention can be applied for obtaining preparations for disinfection of surfaces in premises, sanitary-technical equipment, items patient care, claimed disinfection preparation can also be applied for disinfection and pre-sterilisation cleaning of products of medical purpose, for disinfection and processing hands of medical personnel. Disinfection preparation includes quaternary ammonium compound, boric acid and represents water solution of quaternary ammonium compound, as such it contains diethyldichloropropenylammonium chloride or diethyldiallylammonium chloride, with the following ratio of initial components, wt %: said quaternary ammonium compound - 1.2 wt %, boric acid - 2.3 wt %, water - the remaining part.

EFFECT: invention ensures increase of bactericidal and fungicidal activity with reduction of concentration of working solutions of preparation, extension of action spectrum, including action on mycobacteria.

4 tbl, 1 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: invention refers to medicine. What is described is a composite material which contains a non-organic substance in the form of a layer or a layer ingredient with the non-organic substance leads to form hydrogen cations in contact with an aqueous medium that induces an antimicrobial effect with the substance being produced of MoO2, MoO3, molybdenum carbide, molybdenum nitride, molybdenum silicide, molybdenum sulphide, molybdenum hexacarbonyl and/or molybdenum acetylacetonate.

EFFECT: antimicrobial effect of the composite material is found through time almost with no limit.

32 cl, 3 tbl

FIELD: chemistry.

SUBSTANCE: invention relates to materials and methods for elimination of live target-cells. Material for elimination of live target-cells contains, at least, one insoluble hydrophobic anionic, cationic or amphoteric charged polymer. Said polymer in contact with water-containing environment: a) is a carrier of strongly acidic or strongly basic functional group; b) has pH value lower than 4.5 or higher than 8.0 and c) possesses proton conductivity and/or electric potential, sufficient for efficient disturbance of pH homeostasis and/or electric balance inside closed volume of said cell. Said charged polymer preserves pH value of medium, surrounding said cells. Said material can be regenerated by regeneration of charged polymer, regeneration of buffer capacity of said material, regeneration of proton conductivity of said material. Manufactured product contains said material.

EFFECT: invention makes it possible to regenerate said purpose.

18 cl, 23 dwg, 9 tbl, 14 ex

FIELD: medicine, pharmaceutics.

SUBSTANCE: group of inventions refers to medicine and may be used in hospitals, polyclinics, resort institutions for high level disinfection and sterilisation. A method for preparing a disinfectant provides mixing of liquid ingredients in the form of two solutions immediately before use. One of the solutions contains, wt %: urea peroxyhydrate - 2-16; corrosion inhibitor Korantin PP - 0.5-2; chelating agent Trilon M Liquid - 0.5-2; sulphuric acid for making the pH value of the solution - 0.5-2; deionised water - the rest. The second solution contains, wt %: ethyl acetate - 20-40; acetic acid - 8-11; potassium bichromate 0.1-0.3; sodium silicate - 0.05-0.7; polyethylene oxide - 0.3-3; acetyl caprolactam - the rest. The relation of the first to second solutions makes 70:1 to 500:1.

EFFECT: group of inventions provide the high disinfecting properties of the product, anti-corrosion effect on steel, non-ferrous metals, chromium-nickel coatings; the agent has no damaging action of the objects to be treated, does not decolour cloths, does not fixes organic impurities, does not damage endoscopes and fibre optics, as well as reduces the solution concentration and exposition time on the treated objects.

3 cl, 1 tbl, 1 ex

Disinfectant // 2466743

FIELD: medicine.

SUBSTANCE: disinfectant containing a chlorinated derivative of isocyanuric acid and a gas-yielding mixture comprises a polymer ingredient specified in a group consisting of polyvinyl alcohol, polyacrylic acid and its copolymers, polyvinylpyrrolidone, water-soluble cellulose esters and their mixture in the following proportions, wt %: chlorinated derivative of isocyanuric acid 20-90, polymer ingredient 0.1-5, gas-yielding mixture - the rest. The gas-yielding mixture represents a mixture of base and acid ingredients. The base ingredient of the disinfectant contains alkaline or alkaline-earth salts of carbonic acid or their mixture. As the acid ingredient, the disinfectant contains organic acids, may contain anticorrosion additives, e.g. sodium benzoate, sodium nitrite, calcium formate, zinc compounds. The disinfectant may contain a builder that is a non-ionic surfactant on the basis of oxyethylated derivatives of alcohols, phenols or organic acids, complexons - salts of ethylenediaminotetraacetic acid, a neutral excipient, e.g. sodium phosphate, sodium sulphate, sodium tartrate, sodium acetate.

EFFECT: invention provides preparing the ready storage-stable disinfection solutions containing active chlorine.

6 cl, 15 ex

FIELD: chemistry.

SUBSTANCE: invention relates to agriculture. A pesticide mixture, selected from mixtures of neonicotinoid, pyraclostrobin and metalaxyl or mixtures of neonicotinoid and pyraclostrobin in synergetically effective amounts, provided that in the case of mixtures of neonicotinoid and pyraclostrobin, the neonicotinoid is not acetamiprid or thiacloprid. Synergetically effective amounts of components of said mixture are applied in any desired sequence, simultaneously, and specifically together or separately, or consecutively, in order to improve plant health, for antifungal control or seed protection.

EFFECT: invention increases treatment efficiency.

15 cl, 2 tbl

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