RU2151613C1 - Method of disinfecting agent preparing - Google Patents

Abstract

FIELD: antibacterial preparations. SUBSTANCE: method involves interaction of hexamethylenediamine dihydrochloride with dicyanediamide and hexamethylenediamine at 160 C for 7-10 h. At the first stage product is reprecipitated with 15-25-% aqueous solution of sodium or potassium salt and at the second stage with 10-14-% aqueous solution of sodium chloride at temperature 30 C, not above. To obtained concentrate 26-40-% aqueous solution of dehydroacetic acid sodium salt (pH is 8, not below) and 0.1-1% of polyvinylpyrrolidone (molecular mass is 12 500 Da, not above) are added. Invention can be used for prophylaxis of formation of moldy fungus, yeast, biofilms. EFFECT: enhanced effectiveness against biofilms, increased stability in storage. 3 cl

Description

 The invention relates to disinfectants for various objects, mainly for the food industry, veterinary medicine. Designed to create an assortment of domestic competitive antimicrobial and disinfecting substances, in particular to prevent the formation of molds, yeast, specific microflora of processing plants, in particular biofilms, for antimicrobial protection of food; can be used as antimicrobial additives in paint films, varnishes, water-emulsion paints and varnishes in medicine, veterinary medicine and in everyday life.

 Studies show that currently the equipment of processing enterprises is covered not with individual bacteria and strains, but with biofilms, which are highly resistant to known disinfectants (Dairy Industry, N 3, 1998, pp. 33-34).

 Most studies of the biofilm resistance mechanism to antimicrobial drugs relate to antibiotics, not to disinfectants.

 Bacteria in biofilms are highly resistant to disinfectants.

A known method of obtaining a disinfectant, including the interaction by heating dicyandiamide, hexamethylene diamine and hexamethylene diamine dihydrochloride. The latter is mixed with dicyandiamide and hexamethylenediamine at 150 ^° C for 5 hours, followed by a rise to 170 ^° C and heating at this temperature for 5 hours. Then, the resulting product is reprecipitated with an aqueous solution of sodium or potassium salt (RU 2122866 C1, 10.12.98) .

Tests of a disinfectant obtained in this way in industry have shown:
- a well-known tool does not effectively disinfect real surfaces of equipment at food industry enterprises, in particular dairy, is not efficient enough with respect to existing biofilms at processing enterprises;
- possesses insufficient stability during storage. During storage, gelation occurs. Unstable when cooled;
- the possibility of destruction during prolonged exposure to high temperatures due to local overheating and mechanical stress.

 The objective of the invention is to obtain a disinfectant devoid of the above indicators.

 EFFECT: creation of a method for producing a disinfectant with an extended spectrum of antimicrobial action, with increased efficiency relative to biofilms, which has increased storage stability. The shelf life of water systems is increased without violating their homogeneity.

 At the same time, the surface tension decreases, the wettability improves, the bitterness of the agent decreases, the content of low molecular weight fractions and synthesis residues decreases, the process is simplified.

The technical result is achieved in that the method for producing a disinfectant comprises reacting hexamethylenediamine dihydrochloride with dicyandiamide and hexamethylenediamine at 160 ^° C. for 7-10 hours and subsequent reprecipitation in 2 stages; in the first stage, reprecipitate with an aqueous solution of 15-25% sodium or potassium salt, and in the second stage, reprecipitate with an aqueous solution of 10-14% sodium chloride at a temperature not exceeding 30 ^o C, a concentrate is obtained and an aqueous solution of 26-40% sodium salt is introduced into it dehydracetonic acid with a pH of at least 8 and inject 0.1-1% polyvinylpyrrolidone with a molecular weight of not more than 12500.

 In this case, it is possible to obtain hexamethylene diamine dihydrochloride before mixing with dicyandiamide and hexamethylene diamine by reacting hexamethylene diamine with hydrochloric acid.

 And as a sodium salt, it is possible to use sodium chloride or the sodium salt of dehydracetate acid or sodium citrate.

 The practical implementation of the invention is illustrated by the following examples.

Example 1
Hexamethylenediamine dihydrochloride (HMDA) in an amount of 0.019 kg of dicyandiamide (DCDA) in an amount of 0.0085 kg, hexamethylene diamine (HMDA) in an amount of 0.0116 kg is thoroughly mixed in a 0.1 L conical heat-resistant glass flask. The flask with the mixture is immersed in an oil bath with a temperature of 160 ^o C and incubated for 7 hours. In this case, the mixture is continued to continuously mix until the completion of the process, which is determined by the cessation of ammonia evolution. Then, upon completion of the process, the product is cooled, dissolved in 0.05 L of hot water when heated, then 0.05 L of a 25% aqueous solution of sodium chloride is introduced with continuous stirring, the working stirrer is turned off, it is left to stand for 20-30 minutes, after which the mixture stratifies into two layers. Separate the upper layer, representing a concentrated solution of the finished product from the lower layer - a solution of sodium chloride containing impurities; then the upper layer is washed with fresh portions of a 10% NaCl solution at a temperature of 25 ^o C.

 A concentrate is obtained into which an aqueous solution of 26% sodium salt of dehydracetate acid with a pH of 9 is introduced. Then 0.1% polyvinylpyrrolidone with a molecular weight of 8500 is introduced. The finished product is analyzed for the content of the basic substance, antimicrobial activity, and the content of residual hexamethylenediamine, and the molecular weight is determined by chemical viscosity.

Example 2
0.015 kg of HMDA is placed in a 100 ml flask, then 10 ml of 36% HCl are added to the flask in portions, then 0.085 kg of DCDA is added to the resulting solution with stirring.

The flask was then placed in an oil bath and the mixture was heated at 160 ^° C. with stirring for 10 hours. With stirring, 11.5 g of HMDA was added to the melt obtained. The mixture is continuously stirred.

Then the mixture is reprecipitated with an aqueous solution of 15% sodium salt and the subsequent reprecipitation is carried out with an aqueous solution of 14% sodium chloride at a temperature of 30 ^° C. Dry, a concentrate is obtained, an aqueous solution of 40% sodium salt of dehydracetate acid with a pH of 10 is introduced into it. Then 1% polyvinylpyrrolidone is added. with a molecular weight of 12500.

 Tests have shown that the disinfectant obtained in this way is quite effective in relation to actually existing biofilms and has an increased purity of the product. The possibility of destruction at high temperatures is excluded. The product is stable during storage and exposure to low temperatures.

Claims (3)

1. A method of producing a disinfectant, comprising reacting hexamethylenediamine dihydrochloride with dicyandiamide and hexamethylenediamine at 160 ^° C. for 7-10 hours and then reprecipitating in two stages: on the first, 15-25% sodium or potassium salt is reprecipitated, on the second, reprecipitated with aqueous a solution of 10 - 14% sodium chloride at a temperature not exceeding 30 ^o C, a concentrate is obtained and an aqueous solution of 26 - 40% sodium salt of dehydracetate acid with a pH of at least 8 is introduced into it and 0.1 - 1% polyvinylpyrrolidone is introduced with a mol.m. no more than 12500.  2. The method according to claim 1, characterized in that the hexamethylenediamine dihydrochloride is prepared before mixing with dicyandiamide and hexamethylenediamine by reacting hexamethylenediamine with hydrochloric acid.  3. The method according to claim 1, characterized in that the sodium salt is used sodium chloride, or the sodium salt of dehydracetate acid, or sodium citrate.