RU2267330C1 - Method for obtaining decontaminating preparation - Google Patents

Abstract

FIELD: microbiology, medicine, veterinary science, food industry.

SUBSTANCE: the present innovation deals with industrial branches where quick and reliable decontamination measures are necessary. The suggested preparation for treating different objects should be prepared by the following technique: synthesized potassium fluoride peroxosolvate should be supplemented with ammonium fluoride, non-ionogenic and anionic SAS at the following ratio, weight%: potassium fluoride peroxosolvate 48-89, ammonium fluoride 23.5-5, non-ionogenic SAS 23.5-5, anionic SAS 5-1. The preparation suggested provides high activity being stable at storage both in dried and solution forms.

EFFECT: higher efficiency of application.

3 dwg, 6 ex, 9 tbl

Description

The invention relates to the field of microbiology, medicine, veterinary medicine, food and other industries where fast and reliable decontamination (disinfection) measures are necessary.

Known methods for producing compositions for decontamination based on a large number of compounds of various nature, including based on compounds of chlorine and hydrogen peroxide.

The main disadvantage of decontaminants based on chlorine compounds is the specific odor causing irritation of the mucous membranes, and allergic reactions, high corrosive properties and adverse environmental effects on the environment, since organochlorine compounds can form extremely highly on its objects, especially in wastewater chemical compounds (dioxins), dangerous for humans and warm-blooded animals.

Decontaminating agents based on hydrogen peroxide, especially peroxosolvates, which can be used for decontamination, both in activated and inactivated forms, are deprived of this drawback.

A known method of producing activated solutions with the release of hydrogen peroxide by dissolving a mixture containing acyloxycarboxylic acids (US Patent No. 2701133, MKI A 61 L 13/00). The decontaminating activity of the solutions obtained according to the aforementioned patent with respect to microorganisms exceeded the activity of aqueous hydrogen peroxide solutions.

However, the resulting mixture during storage is able to agglutinate, which leads to a loss in the content of active substance. In addition, in the recommendations on the introduction of various additional compounds for water binding in order to avoid agglutination of the mixture in an amount of 0.5 ... 80 weight%, optimally 2 ... 50 weight%, it can potentially worsen the toxicological properties of disinfecting and decontaminating solutions, as proposed the inclusion of such compounds as salts of aromatic sulfonic acids (benzene, toluene, xylene, cumene sulfonic acids).

From the point of view of the current environmental situation and with the toughening of the requirements for disinfectants, it is inappropriate to recommend widespread use of derivatives of aromatic hydrocarbons in the proposed amounts, in terms of their biodegradability and toxicity.

There is a method of producing compositions in which potassium fluoride, urea, sodium carbonate peroxohydrates are used as compounds releasing hydrogen peroxide in a solution (AS USSR No. 1152115, A 61 L 2/16). Solid carriers of hydrogen peroxide (peroxohydrates (peroxosolvates) of salts of various metals) have a number of advantages over hydrogen peroxide solutions. They have a wide spectrum of antimicrobial action, good storage stability both in dry form and in the form of aqueous solutions.

However, to achieve a sporocidal effect, solutions with a content of hydrogen peroxide of 4.5-6.0% are recommended for use, which corresponds (in the case of PFC-1) to 13-17% for the compound. The use of peroxohydrate solutions at the indicated concentrations leads to the appearance of salt on the treated surfaces, which, although it is easily washed off, however, this leads to an additional operation. Therefore, to reduce the concentration of the compound, it is necessary to introduce additives that would achieve a sporocidal effect with a lower content of potassium fluoride peroxosolvate in the working solution.

The closest analogue in technical essence and the achieved positive result to the claimed technical solution is the "Method of obtaining a decontaminating agent based on hydrogen peroxide and / or peroxosolvates." The method is obtained by mixing the activator with chemicals or mixtures thereof, and hexamethylenetetramine, or diphenylamine, or trilon-B, or carbamide, or carboxylic acids are used as the activator at a ratio of hydrogen peroxide in the carrier to the activator 99.0-99.5: 0 , 5-1.0 wt.% (See RF patent No. 204275, MKI A 61 L 2/16).

The disadvantage of the prototype is that the activators are introduced at the time of peroxosolvate synthesis into the mother liquor, where the process of formation of active centers that can increase the sporocidal activity of the obtained decontaminating agent occurs. However, when the solvent is distilled off in a rotary-film evaporator, quite stringent conditions are created under which part of the active sites can be destroyed, which leads to a possible decrease in the sporocidal effect of the introduced additives and a decrease in the product resistance.

The technical result of the proposed technical solution is the creation of a more active decontaminating agent based on peroxosolvates, by introducing additional components into the synthesized peroxosolvate.

The technical result is achieved by the fact that ammonium fluoride, nonionic and anionic surfactants are introduced into the synthesized potassium fluoride peroxosolvate in the following ratios, wt.%:

potassium fluoride peroxosolvate 48-89 ammonium fluoride 23.5-5 nonionic surfactant 23.5-5 anionic surfactant 5-1

A significant difference of the proposed solution is that the components are introduced into the synthesized peroxosolvate after it leaves the rotary film evaporator (after distillation of the evaporator) and the formation of active centers occurs in a dry mixture, and the components interact with each other with the formation of new active centers.

When ammonium fluoride is introduced into the synthesized peroxosolvate, a potassium acid fluoride peroxosolvate is partially formed, which has a greater decontaminating activity compared to potassium fluoride peroxosolvate, which is clearly illustrated in the radiographs presented.

Figure 1 presents the x-ray peroxosolvate of potassium fluoride.

Figure 2 - x-ray sample of peroxosolvate potassium fluoride, in the mother liquor for the synthesis of which was made 10% NH ₄ F.

Figure 3 presents the x-ray of a mixture of potassium fluoride peroxosolvate and 10% NH ₄ F. In this x-ray, peaks are clearly visible that characterize the presence in the structure of acid potassium fluoride, which are absent in figures 1 and 2.

From the presented X-ray diffraction patterns it is seen that the mixture of PFC and NH ₄ F has a more stable structure, which was confirmed by monitoring the stability of these drugs.

In addition, with the simultaneous introduction of nonionic and anionic surfactants, the decontaminating properties are enhanced by increasing the wettability of the treated surface and thereby improving the contact of the decontaminating agent with the treated surface.

We experimentally established the components of the decontaminating agent (see table 1) and their quantitative ratios necessary to achieve the optimal positive effect. Succinic acid is shown in the examples as a nonionic surfactant, and a compound with the commercial name "Nioxol" is used as anionic surfactant.

Table 1
Dependence of the constants of the kinetics of inactivation of spores of you. cereus, var anthracoides pcs. 250 from the composition of the decontaminating agent. The composition of the decontaminating agent, g K ', sp · ml ^-1 · min ^-1 K "(for H ₂ O ₂ ),
cn · ml ^-1 · min ^-1 · mol ^-1 potassium fluoride peroxosolvate 48; ammonium fluoride 23.5; 0.1689 ± 0.0238 0.7460 ± 0.1051 succinic acid 23.5; surfactant 5. ammonium fluoride 23.5; succinic acid 23.5; 0.0081 ± 0.0044 - surfactant 5. potassium fluoride peroxosolvate 48; ammonium fluoride 23.5; 0.1322 ± 0.0129 0.5579 ± 0.0503 succinic acid 23.5. potassium fluoride peroxosolvate 48; ammonium fluoride 23.5; 0.0659 ± 0.0025 0.2754 ± 0.0093 surfactant 5. potassium fluoride peroxosolvate 48; succinic acid 23.5; 0.1549 ± 0.0009 0.6542 ± 0.0041 surfactant 5.

Conclusion: a higher decontaminating activity against spores of a test object of a stable form of microorganisms in comparison with potassium fluoride peroxosolvate is inherent in all compositions listed in table 1. However, the composition with the ratio of the components shown in the first top row of Table 1 is most active, which is illustrated by the highest value of the spore inactivation kinetics constant, which characterizes the speed of the decontamination process.

Example 1

48 g of potassium fluoride peroxosolvate were taken, 23.5 g of ammonium fluoride and 23.5 g of nonionic surfactant, in particular succinic acid, were added to it, then 5 g of liquid anionic surfactant ("Nioxol") was added, mixed.

A 10% aqueous solution was made from the resulting dry mixture based on the total weight of the decontaminating agent. The content of hydrogen peroxide in the resulting solution was 1.5%.

Then, the kinetics constant of inactivation of spores of Vas. cereus, var anthracoides pcs. 250 was experimentally determined. 10 ml of a spore suspension of Vascereus, var anthracoides pcs. 250, prepared previously, and 10 ml of a 10% working solution of a decontaminating agent were taken into a 50.0 ml flask. The flask was placed on a magnetic stir bar for stirring at a constant speed. From it, after 15 minutes, 105 ml were taken for 105 minutes in a neutralizer solution. The sample was triturated according to the generally accepted method when working with microorganisms. Next, from each dilution, 2 samples of 1 ml were sown per Petri dish, poured with meat and peptone agar and placed in a thermostat for 24-48 hours, after which time the number of grown colonies in each cup was counted. The experimental data were statistically processed. The data obtained are presented in table 2.

table 2
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Cereus, var anthracoides pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 16.70 ± 0.36 0.3170 1.89 fifteen 16.48 ± 0.01 0.0490 0.29 thirty 15.13 ± 0.21 0.2423 1,60 40 12.29 ± 0.48 0.5412 3.41 fifty 9.16 ± 0.31 0.2654 1.65 60 7.14 ± 0.077 0.4581 6.41

K '= 0.1689 ± 0.0238 cn · ml ^-1 · min ^-1

K "(for H ₂ O ₂ ) = 0.7460 ± 0.1051 cn · ml ^-1 · min ^-1 · mol ^-1

Example 2

23.5 g of ammonium fluoride were taken, 23.5 g of nonionic surfactant, in particular succinic acid, was added, then 5 g of liquid anionic surfactant ("Nioxol") was added, mixed.

Next, the kinetics constant of the inactivation of spores of you.cereus, var anthracoides pcs. 250 was determined in the same way as in example 1.

Table 3
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Cereus, var anthracoides pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 17.92 ± 0.10 0.1650 0.92 fifteen 17.74 ± 0.01 0.0450 0.25 45 17.33 ± 0.12 0.1800 1,03 75 17.23 ± 0.10 0,1605 0.95 90 17.14 ± 0.46 0.3550 2.07 105 14.05 ± 0.07 0.1350 0.79

K '= 0.0081 ± 0.0044 sp · ml ^-1 · min ^-1

Example 3

48 g of potassium fluoride peroxosolvate were taken, 23.5 g of ammonium fluoride was added to it, 5 g of anionic surfactant was added, in particular, Nioxol, and mixed.

Next, the kinetics constant of inactivation of spores of Vas.cereus, var anthracoides pc. 250 was determined analogously to example 1.

Table 4
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Cereus, var anthracoides pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 18.16 ± 0.02 0,0700 0.39 fifteen 17.33 ± 0.53 0.3800 2.19 45 16.21 ± 4.52 1,1100 6.84 75 14.72 ± 0.84 0.4800 3.26 90 13.23 ± 0.36 0.3150 2,38 105 10.28 ± 0.05 0.0528 1.16

K '= 0.0659 ± 0.0025 cn · ml ^-1 · min ^-1

K "(for H ₂ O ₂ ) = 0.2754 ± 0.0093 cn · ml ^-1 · min ^-1 · mol ' ¹

Example 4

48 g of potassium fluoride peroxosolvate were taken, 23.5 g of ammonium fluoride was added to it, 23.5 g of nonionic surfactant, in particular succinic acid, was added, mixed.

Next, the kinetics constant of the inactivation of spores of you.cereus, var anthracoides pcs. 250 was determined in the same way as in example 1.

Table 5
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Cereus, var anthracoides pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 18.08 ± 0.08 0.1500 0.83 fifteen 17.34 ± 0 0 0 45 13.87 ± 4.68 1,1300 8.1470 75 8.57 ± 4.20 1,0700 12.48 90 6.84 ± 0.49 0.3650 5.33 105 4.93 ± 5.64 1,2400 9.12

K '= 0.1322 ± 0.0129 sp · ml ^-1 · min

K "(for H ₂ O ₂ ) = 0.5579 ± 0.0503 cn · ml ^-1 · min ^-1 · mol ^-1

Example 5

48 g of potassium fluoride peroxosolvate were taken, 23.5 g of nonionic surfactant, in particular succinic acid, were added, then 5 g of liquid anionic surfactant ("Nioxol") was added, mixed.

Next, the kinetics constant of inactivation of spores of Vas.cereus, var anthracoides pc. 250 was determined analogously to example 1.

Table 6
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Cereus, var anthracoides pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 18.08 ± 0.08 0.1500 0.83 fifteen 16.59 ± 0.04 0,1100 0.66 45 13.66 ± 0.13 0.1900 1.39 75 5.65 ± 0.44 0.3450 6.11 90 5.30 ± 0.53 0.3800 2.19 105 0 0 0

K '= 0.154910,0009 cn · ml ^-1 · min

K "(for H ₂ O ₂ ) = 0.6542 ± 0.0041 cn · ml ^-1 · min ^-1 · mol ^-1

Example 6

89 g of potassium fluoride peroxosolvate were taken, 5 g of ammonium fluoride and 5 g of nonionic surfactant, in particular succinic acid, were added to it, then 1 g of liquid anionic surfactant ("Nioxol") was added, mixed.

Next, the kinetics constant of the inactivation of spores of you.cereus, var anthracoides pcs. 250 was determined in the same way as in example 1.

Table 7
Statistically processed data of experiments to determine the constants of the kinetics of inactivation of spores of you. Anthracoides, var cereus pcs. 250. Inactivation time, τ min The average value (ln) of the number of surviving spores by time τ Confidence Interval σ Coefficient of variation V,% 0 16.70 ± 0.37 0.3170 1.89 fifteen 16.38 ± 0.37 0.3174 1.93 thirty 15.38 ± 0.04 0.1055 0.69 40 13.69 ± 2.22 0.7786 5.68 fifty 10.63 ± 1.37 0.6120 5.75 60 6.81 ± 0.07 0.1375 2.02

K '= 0.1575 ± 0.0020 cn · ml ^-1 · min ^-1

K "(for H ₂ O ₂ ) = 0.3810 ± 0.0060 cn · ml ^-1 · min ^-1 · mol ^-1

The obtained decontaminants are stable both in dry form and in the form of a working solution.

The decontaminating agent we obtained was stored at room temperature. After certain time intervals (1, 2, 3, 4, 7, 14, 28, 52, 64, 72 days), samples were taken and the content of hydrogen peroxide was determined in them. The obtained data on the stability of the dry mixture of decontaminating agents are presented in table 8.

Table 8
Change in the content of hydrogen peroxide in a dry mixture of decontaminating agent during storage. Shelf life, days The content of N ₂ About ₂ ,% The decomposition coefficient,% / day 0 14.45 ± 0.02 one 15.01 ± 0.01 -0.5600 2 14.87 ± 0.01 -0.2100 3 15.39 ± 0.02 -0.3133 four 15.28 ± 0.05 -0.2075 7 15.03 ± 0.05 -0.0829 fourteen 14.87 ± 0.03 -0.0300 28 14.25 ± 0.07 0.0071 52 13.23 ± 0.12 0,0235 64 12.11 ± 0.02 0,0366 74 12.18 ± 0.09 0,0307 * - "-" characterizes the increase in the content of hydrogen peroxide.

At the same time, 10% solutions (100 ml) of the obtained decontaminating agent were prepared, which were analyzed similarly to a dry mixture for the content of hydrogen peroxide during storage. The obtained data on the stability of the solutions are presented in table 9.

Table 9
The stability of the disinfectant solution when stored in a plastic container. Shelf life, days The content of H ₂ About ₂ ,% The decomposition coefficient,% / day 0 1,50 ± 0,02 - one 1.49 ± 0.02 0.010 2 1.47 ± 0.01 0.015 3 1.47 ± 0.01 0.010 four 1.47 ± 0.02 0.0075 7 1.48 ± 0.01 0.0029 fourteen 1.42 ± 0.02 0.0057 28 1.38 ± 0.03 0.0043 52 1.22 ± 0.01 0.0054 64 1.14 ± 0.01 0.0056 74 1.07 ± 0.01 0.0058

As can be seen from tables 8 and 9, we obtained decontaminating agent is stable during storage both in dry form and in the form of a solution.

Claims (1)

A method of obtaining a decontaminating agent based on peroxosolvates by mixing them with chemicals or mixtures thereof, characterized in that ammonium fluoride, nonionic and anionic surfactants are introduced into the synthesized potassium fluoride peroxosolvate in the following ratio, wt.%: Potassium Fluoride Peroxosolvate 48-89 Ammonium fluoride 23.5-5 Nonionic surfactant 23.5-5 Anionic surfactant 1-5

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