Stable peracetic acid aqueous solution with scale removal property, for use in CIP systems in the food, dairy, and beverage industries

Abstract

This invention is related to the preparation of commercial acid sanitizing and / or cleaning compositions comprising peracetic acid with antimicrobial and descaling properties at the same time. The present invention is used in CIP (cleaning in place) systems in the food, dairy, and beverage industries, as well as heating and cooling circulating water systems in all industries.

Description

Stable peracetic acid aqueous solution with scale removal property, for use in CIP systems in the food, dairy, and beverage industries

[0001] This invention is related to the preparation of commercial acid sanitizing and / or cleaning compositions comprising peracetic acid with antimicrobial and descaling properties at the same time. The present invention is used in CIP (cleaning in place) systems in the food, dairy, and beverage industries, as well as heating and cooling circulating water systems in all industries.

[0002] C11D 3 / 48

[0003] CN102037959B- Method for preparing stable peracetic acid disinfectant

[0004] The invention relates to a method for preparing stable peracetic acid disinfectant. The peracetic acid disinfectant comprises the following raw materials in percentage by weight: 27% to 39% of hydrogen peroxide, 22% to 36% of acetic acid, 0.01% to 2% of composite stabilizer, 0.01% to 2% of surfactant, and the balance of water. In the obtained peracetic acid disinfectant, the mass concentration of peracetic acid is 15 to 20g / 100g, the mass concentration of the hydrogen peroxide is 20 to 30g / 100g, and the mass concentration of the acetic acid is 10 to 20g / 100g. The peracetic acid disinfectant prepared by the method has the characteristics of a high concentration of peracetic acid, good stability, good disinfection, and sterilization effect, a simple production process, safety, and the like.

[0005] The invention above discloses a disinfectant composition comprising hydrogen peroxide, acetic acid, stabilizer, surfactant, and water balance in percentage by weight. The concentration of peracetic acid in the final solution is 15 to 20% by weight, and the concentration of the hydrogen peroxide is 20 to 30% by weight. The peracetic acid disinfectant prepared by this method does not have descaling properties and is only used as a disinfectant. Also, it differs from the present invention in its percentages and ingredients.

[0006] KR20210041899A- Solid Peracetic Acid Disinfectant

[0007] The present invention relates to a peracetic acid disinfectant for sterilization and disinfection, and more specifically, to a solid peracetic acid disinfectant which is very advantageous in handling and transportation by being in a solid form such as granules or tablets, unlike conventional liquid peracetic acid and hydrogen peroxide disinfectants. The solid peracetic acid disinfectant contains acetyl compounds and percarbonate.

[0008] The mentioned invention discloses a peracetic acid disinfectant for sterilization and disinfection, and more specifically, a solid peracetic acid disinfectant which is very advantageous in handling and transportation by being in a solid form such as granules or tablets, unlike conventional liquid peracetic acid and hydrogen peroxide disinfectants. The solid peracetic acid disinfectant contains acetyl compounds and percarbonate. This formulation is in a solid form with different ingredients. Besides, It has a disinfecting function, not a descaling one.

[0009] US5330769A- Acid sanitizer

[0010] Fatty acid sanitizer concentrates and diluted final solutions are provided which include individual amounts of germicidally effective fatty acid, hydrotrope, strong acid sufficient to lower the pH of the final solutions to about 1-5, and a concentrate stabilizing weak acid component selected from the group consisting of propionic, butyric and valeric acids and mixtures thereof. The concentrate stabilizing component enhances the room and low temperature phase stability of the concentrates, even when used at very low steps typically ranging from 2.5%-15% by weight. Preferably, the fatty acid is a mixture of nonanoic and decanoic acids, whereas the strong acid is selected from the group consisting of orthophosphoric, sulfuric, and mixtures thereof.

[0011] The invention above discloses fatty acid sanitizer compositions in both concentrated and diluted forms with stabilizing agents. The formulation of this invention includes an effective amount of a weak acid selected from the group consisting of propionic, butyric, and valeric acids and mixtures. Also, the fatty acid is a mixture of nonanoic and decanoic acids, whereas the strong acid is selected from the group consisting of orthophosphoric, sulfuric, and mixtures thereof. The formulation of this invention does not contain peracetic acid as a disinfectant, unlike the present invention. Also, nitric acid is not used as a descaling agent.

[0012] US4404040A- Short chain fatty acid sanitizing composition and methods

[0013] Sanitizing concentrate and "use" compositions comprising aliphatic, short chain fatty acid (i.e., C6 -C14 fatty acid), hydrotrope or solubilizer for the fatty acid, hydrotrope-compatible acid so that the concentrate, when diluted with a major amount of water provides a use solution having a pH in the range of 2.0 to 5.0. Sanitizing of substantially fixed, "in-place" processing lines in dairies, breweries, and other food processing operations is a particular utility of this invention.

[0014] The invention above discloses cleaner and sanitizer compositions containing fatty acid, hydrotrope, or solubilizer for the fatty acid and hydrotrope-compatible acid. Although the formulation made in this patent has the same application as the present invention, but all the raw materials used in this patent are different, and peracetic acid as a disinfectant, as well as organic and inorganic acids such as acetic, phosphoric, and nitric, are not used.

[0015] US3867300A- Bactericidal composition

[0016] The present invention relates to compositions having surprising bactericidal activity. The compositions of the present invention are aqueous compositions containing from 5 to 15 percent of an aliphatic monocarboxylic acid having from 8 to 11 carbon atoms, and the balance is either a non-ionic or anionic detergent.

[0017] The invention above relates to compositions having bactericidal activity. The compositions of the present invention are aqueous compositions containing an aliphatic monocarboxylic acid and a non-ionic or anionic detergent. However, peracetic acid is not used in this patent and the mentioned formulation can only be used as a bactericide and has no descaling property.

[0018] US6472358B1- Acid sanitizing and cleaning compositions containing protonated carboxylic acids

[0019] A sanitizing composition comprising at least one aliphatic short chain antimicrobially effective C5 to C14 fatty acid or mixture thereof, at least one carboxylic weak acid, and a strong mineral acid which may be nitric or a mixture of nitric and phosphoric acids.

[0020] The invention above discloses acid Sanitizing and / or cleaning compositions comprising carboxylic acids, fatty acids, mineral acids, surfactants, and hydrotropes. Although In the formulation of this patent, nitric or phosphoric acid has been used to increase the descaling and cleaning properties along with other weak carboxylic acids, but its disinfectant base does not contain peracetic acid. Also, in the formulation of this patent, anionic surfactants are used, but the current patent does not use any surfactants.

[0021] US20060035808A1- non-chlorinated concentrated all-in-one acid detergent and method for using the same

[0022] Non-chlorinated concentrated acid detergent compositions and methods for using the same are provided. More particularly, the acid detergents comprise a quantity of a fatty alkyl-1,3-diaminopropane or salt thereof and optionally alkylsulfonic acid. The detergents form the basis for an all-in-one cleaning, sanitizing, and sediment removal composition for use on soiled surfaces, particularly surfaces contaminated with milk soils and other food soils.

[0023] The mentioned invention discloses concentrated acid detergent compositions and methods of using the composition, either as a concentrate or as a diluted use solution, to clean, sanitize, and remove scale from a soiled surface. More particularly, the acidic detergent compositions according to the present invention comprise organic and inorganic acid, hydrotrope, surfactant and enzyme. The formulations of this patent, like the current patent, are designed to perform both cleaning and disinfection operations at the same time. Also, it is suitable for separating the contamination of milk from food contact surfaces, but it is different in terms of formulation and the type of raw materials used in the formulation, and surfactant is also used in the formulation of this patent.

[0024] US5998358A- Antimicrobial acid cleaner for use on organic or food soil

[0025] The invention relates to compositions and methods for cleaning typically organic beverage and food soils. The cleaning composition is formulated to remove carbohydrate and proteinaceous soils from hard surfaces. The formulations of the invention are directed to remove carbohydrate and proteinaceous soils from beverage manufacturing locations such as soils arising in the manufacture of malt beverages, fruit juices, dairy products, etc.

[0026] The invention above relates to acid-cleaning compositions formulated for organic Soil removal or, more particularly for food Soil removal. Further, the invention relates to cleaning processes to remove carbohydrate and proteinaceous soils from beverage manufacturing locations use a clean-in-place method. The formulation of this patent includes phosphoric acid, organic acids, solvents, stabilizers, and surfactants such as quaternary ammonium compounds. There is no peracetic acid in the prepared formulation and the obtained solution has low foaming properties, which limits its use for circulation systems in the food, beverage, and dairy industries.

[0027] US6867233B2- Acidic antimicrobial compositions for treating food and food contact surfaces and methods of use thereof

[0028] Acidic antimicrobial compositions for treating food surfaces and food contact surfaces comprise an organic acid and a surfactant, said composition having a pH of from about 2 to about 5. Concentrated, acidic antimicrobial compositions preferably comprise a stabilizing agent to prevent precipitation of the surfactant upon dilution of the concentrated composition. Methods of use comprise contacting food surfaces or food contact surfaces with the compositions of the present invention. Articles of manufacture comprise a container, an acidic antimicrobial composition, and a set of instructions in association with the container.

[0029] The patent uses phosphoric acid along with methane sulfonic acid and other additives such as various surfactants, which focus more on the cleaning ability of the formulation, and the surfactants used in the formulation can create foam in the circulation system, especially when the dosage is increased.

[0030] US20180187129A1- Acid detergent

[0031] Acid detergent compositions, concentrates and use solutions prepared from the concentrates and methods of using the same are provided. The acid detergent compositions are particularly suited for use in removing soils, especially milk soils, from clean-in-place systems, such as those commonly used in the dairy and food processing industries. The detergent compositions comprise an acidic component including an inorganic or alkanesulfonic acid and a blend of surfactants to provide high cleaning efficiency and low foam generation. The acid detergent compositions optionally comprise an antimicrobial agent to impart a sanitization functionality to the detergent.

[0032] The invention above, is a combination of organic and inorganic acids such as phosphoric acid, citric acid, acetic acid, sulfamic acid, and sulfuric acid are used along with various surfactants. Generally, the organic acids and surfactants used in these formulations increase the price of the formulation, especially the amount required for dilution of these formulated products is not small. Also, the chemical base used for disinfection in the formulations of the mentioned patents is not peracetic acid.

[0033] US8685173B2- Method of cleaning food and beverage manufacturing and handling equipment

[0034] The present invention is generally directed toward methods of cleaning and sediment removal of surfaces contaminated with food soils, especially clean-in-place systems. More particularly, the methods according to the present invention also provide for sanitizing of surfaces contaminated with food soils. Thus, there is provided a single cleaning cycle that may clean, sanitize, and descale food-soiled surfaces, and in certain embodiments, without the need for a pre-rinse step, using an acidic detergent composition comprising a fatty alkyl-1,3-diaminopropane or salt thereof in the presence of an acid selected from the group consisting of inorganic acids, organic acids, and mixtures thereof.

[0035] The mentioned invention patent uses phosphoric acid along with methane sulfonic acid and other additives such as various surfactants, which focus more on the cleaning ability of the formulation, and the surfactants used in the formulation can create foam in the circulation system, especially when the dosage is increased.

[0036] The use of mineral acids such as sulfuric acid, nitric acid or methane sulfonic acid along with peracetic acid is not necessary to create cleaning or descaling properties. For example, nitric acid is used in a small amount in order to limit the corrosion problems of peracetic acid on stainless steel surfaces, and the added amount does not have the ability to descale. Also, the formulation made in this patent is completely different from the present patent in terms of the percentage of compounds

[0037] US4587264A- Disinfection and sterilizing solution of peracetic acid and nitric acid

[0038] Commercial solutions of noncorrosive and time-stable carboxylic peracids, particularly peracetic acid, contain an acid of oxidizing nature, such as nitric acid, present in a weight percentage at least equal to that of the carboxylic peracid. Such solutions, diluted with ordinary water, are useful for the sterilization and microbiological disinfection of asceptic enclosures, and of equipment of the food industry, particularly the milk industry, with reduced risk of corrosion to the equipment.

[0039] The invention above The use of mineral acids such as sulfuric acid, nitric acid or methane sulfonic acid along with peracetic acid is not necessary to create cleaning or descaling properties. nitric acid is used in a small amount in order to limit the corrosion problems of peracetic acid on stainless steel surfaces, and the added amount does not have the ability to descale. Also, the formulation made in this patent is completely different from the present patent in terms of the percentage of compounds.

[0040] US8822719B1- Peroxycarboxylic acid compositions suitable for inline optical or conductivity monitoring

[0041] Peracid stable fluorescent active compounds in highly acidic, equilibrium peroxycarboxylic acid sanitizing compositions are disclosed as having improved fluorescent stability allowing for monitoring of peroxycarboxylic acid concentration by conductivity and / or optical sensors. Beneficially, the compositions are also low odor and low / no VOC dual functioning acid wash and sanitizing compositions.

[0042] In the mentioned invention, sulfuric acid is used as a mineral acid along with peracetic acid. The purpose of adding sulfuric acid in this patent is to increase the acidic conditions in terms of pH and also to increase the reaction speed in the two-way reaction of peracetic acid production. Anyway, the formulation of this patent is different from the present patent, so besides peracetic acid, there is also the combination of per octanoic acid with surfactant.

[0043] The composition includes Peracetic acid, Nitric acid, Acetic acid (glacial), Hydrogen peroxide, Phosphoric acid, HEDP, deionized water, and stabilizer. The descaling power of the composition depends directly on the amount of Acetic acid in it. The nitric acid in the formulation helps descaling and disinfection to happen simultaneously. Simultaneous disinfection and descaling reduce the CIP stages. For the CIP stages to be less, the composition contains no surfactant, therefore no rinsing is needed in the final stage.

[0044] cleaning and sanitation are two crucial stages in food production factories, which are routinely performed at the end of food production operations. In the production of spoilable food and sensitive to microbial contamination, this operation is extremely important and may be done in the middle of production in addition to the end of each work shift. These conditions also exist in the production of beverages and the cleaning and sanitation steps are carried out carefully. Antimicrobial stages, as well as cleaning stages, are therefore required for all critical surfaces to reduce microbial populations to safe levels established by public health regulations. This process is generally referred to as sanitizing.

[0045] CIP (cleaning in place) is a common cleaning method in which both alkaline and acidic cleaners are used to remove all types of visible contaminations. These visible contaminants mainly include organic compounds such as fat, protein, and sugar, which are removed using alkaline cleaners. Sodium hydroxide, potassium hydroxide, and formulated alkaline cleaners are different examples of these alkaline compounds.

[0046] Inorganic compounds are another form of visible contamination that includes all kinds of mineral deposits from food or water hardness that are removed by acidic formulations. These mineral deposits are known as milkstone in dairy factories, which contain a large amount of calcium phosphate and are difficult to remove from the surface of the equipment. Also, mineral deposits resulting from water hardness, including calcium carbonate and magnesium are other common sticky deposits in the dairy, food, and beverage industries that are formed on the surface due to the temperature, alkalinity, or in reaction with foods. Nitric acid, phosphoric acid, and formulated acidic cleaners can be used to remove these mineral contaminations in the acidic cleaning step. It is expected that at the end of the cleaning process, all the visible contaminations are removed from the surface so the disinfection step can be carried out in the best way.

[0047] sanitation is the level at which invisible contamination such as microorganisms are removed from the surfaces. sanitation is done with two thermal and chemical methods. Using chemical sanitizing solutions is expanded today, due to many advantages. Different sanitizer compounds can be used at this stage, which can be compared based on various aspects. corrosive on the stainless steel and polymer, board spectrum antimicrobial action, stability in concentrate and ready-to-use status, the resistance of the microorganisms to the sanitizing solution, the toxic residue of sanitizer after usage, cost-effective and the pH effect on the antimicrobial action are the most important factors for choosing the proper sanitizer. chlorine compounds such as Sodium hypochlorite, quaternary ammonium compounds such as Benzalkonium chloride and didecyldimethylammonium chloride, peracid compounds such as peracetic acid and peroctanoic acid, organic acids such as citric acid and caprylic acid with surfactants are some of the common sanitizers in the food, dairy, and beverage industries.

[0048] But one of the important features of choosing a sanitizer is that it does not need to be rinsed at the end of the CIP operation. One of the advantages of this important feature is the reduction of the water consumption amount in the CIP operation. By choosing a proper sanitizing solution that has no toxic residue, the final rinsing step in the CIP operation is eliminated, which plus less water consumption, reduces the time of the CIP operation.

[0049] The FDA (The United States Food and Drug Administration) in CFR.178.10.10 has clarified the disinfectant compounds that can be used on food contact surfaces that do not require rinsing Among these compounds, the name of peroxyacetic acid is mentioned in a dose of 150 to 200 ppm. Peroxyacetic acid is a broad-spectrum sanitizer that decomposes into water and CO2 (carbon dioxide) and leaves no dangerous residue.Solution of problem

[0050] Paracetic acid is one of the peracid compounds that is synthesized from the reversible reaction between acetic acid and hydrogen peroxide. In this method, after the reaction between acetic acid and peroxide hydrogen, the peracetic acid and water are produced, and due to the reversibility of this reaction, some of the ingredients of the reaction remain in the final product. As a result, we can say that after the reaction reaches equilibrium, the peracetic acid, acetic acid, hydrogen peroxide, and water are present in the final product.

[0051] As a very strong sanitizing composition and disinfectant, peroxyacetic acid is effective against a broad spectrum of microorganisms and despite many disinfectants, it does not contain dangerous and harmful residues. For this reason, the FDA has approved this compound for use in food and dairy industries for food contact surfaces.

[0052] It is stated in CFR 178.I0.I0 that if the final concentration of peroxyacetic acid in the final sanitizing solution is less than 200 ppm on the surfaces directly in contact with the food, there is no need to rinse. Peroxyacetic acid and other raw materials used to make it turn into carbon dioxide and water after decomposition, which shows that peroxyacetic acid does not leave a dangerous residue.

[0053] However, one of the main problems of peracetic acid is its instability which causes the need to use stabilizing compounds. In the case of not using a stabilizer in the formulation, the synthesized peracetic acid is decomposed and decreased in a short time. Peroxyacetic acid remains stable for 12 to 18 months using stabilizers. If the percentage of synthesized peroxyacetic acid in the final product is high, it becomes more difficult to keep it stable over time. The 1,1 Hydroxyethylidene phosphonic acid (HEDP), Ethylenediaminetetraacetic acid (EDTA), phosphate compounds like Tetrasodium pyrophosphate and phosphoric acid, quinoline derivatives, and 2,6-pyridine dicarboxylic acid are the proper stabilizers for the peracetic acid.

[0054] Although various researches have been carried out over the past years to optimize the performance of alkaline cleaners, acid cleaners, and disinfectants separately in different stages of CIP, research on reducing CIP stages to reduce the time of the CIP process, which can lead to a reduction in water consumption It can be very useful. Although the use of peroxyacetic acid as a disinfectant in the CIP process eliminates the need for final rinsing, it is desirable to combine the two steps of the CIP process to reduce the number of stages.

[0055] Considering the nature of organic and inorganic contaminations and their solubility which are dissolved in alkaline and acidic detergents, it is not easy to combine the two alkaline and acidic stages, and it increases the risk of the presence of visible residue and negative effects on the sanitizing solution performance. However, a limited number of formulated compounds are commercially available with this feature. However, the combination of the acid cleaning and disinfection stage, especially when the sanitizer is selected with an acidic nature, is probable.

[0056] The composition of the present invention is an acid-sanitizer solution used to remove mineral deposits and sanitation and reduce the microbial load in the CIP process.

[0057] The sanitizing and cleaning compositions of the present invention perform descaling and sanitation operations at the same time.

[0058] The composition of the present invention does not contain fatty acids and surfactants, and as a result, it does not create any foam during use and is suitable for the CIP process.

[0059] In the composition of the present invention, all the raw materials have proper dissolution and compatibility with the formulation. As a result, during the storage, it has phase stability and remains a single-phase solution.

[0060] The composition of the present invention does not contain organic acids such as decanoic acid, nonanoic acid, and butyric acid, so it has a reasonable price from an economic point of view.

[0061] The composition of the present invention has a suitable amount of peracetic acid as a sanitizer and suitable mineral acids such as nitric and / or phosphoric acid for descaling, which results in incredible performance after dilution and use in the CIP process.

[0062] The composition of the present invention contains nitric acid or phosphoric acid as a descaling agent, which together with acetic acid, which is needed in the formulation of peracetic acid, performs the removal of mineral deposits.

[0063] The composition of the present invention contains peracetic acid and mineral acids such as nitric or phosphoric acids used in CIP systems in the food, dairy, and beverage industries.

[0064] peracetic acid is a proper disinfectant with a broad-spectrum antimicrobial that is very common in the food and dairy industries. Hydrogen peroxide and acetic acid are used as two primary ingredients in the formulation of peracetic acid.

[0065] Using acid-sanitizers as formulations that have two simultaneous functions at the same time and can be used in the CIP process and reduce the CIP stages. By using these formulations, the two-acid cleaning and sanitation stages are merged and the CIP time can be reduced.

[0066] Formulated compounds in previous patents that could perform descaling and disinfection, had formulas with different percentages of different materials. In the previously produced acid-disinfectant formulations including Agrochem CO. ( Oxystrike ), Envirotech CO. ( reflex ), and Spraychem CO. ( save a step ), the formulation contains 1 to 5% acetic acid, 5 to 7% peracetic acid, 21 Up to 24% hydrogen peroxide, and 7-10% nitric acid. In the above formulations, nitric acid has been used as a descaler, but the use of other acids such as phosphoric acid can also be investigated. The [Table. 1] illustrates the percentage of ingredients of the above three commercial formulations.

[0067] Also, in the above formulations, the amount of acetic acid remaining in the formulation after equilibrium is 1 to 5%, a large amount of which has been used for the synthesis of peracetic acid, and it is possible to improve and increase the amount of acetic acid in the formulation from the remaining amounts. The residual acetic acid was used in the formulation and the descaling power of the formula was increased by using acetic acid together with nitric or phosphoric acid. In fact, it can be said that by increasing the amount of acetic acid in the process of peracetic acid synthesis and reducing the amount of hydrogen peroxide in the formulation, the remaining acetic acid is optimally used to increase descaling ability. In fact, by increasing the amount of acetic acid in the formulation of this invention, a small part of it is used for the production of peracetic acid, and the rest of it is used for the descaling of mineral deposits and helps nitric acid and phosphoric acid. so that descaling operations can be done better and more.

[0068] Acid-sanitizer composition of the present invention comprises hydrogen peroxide, acetic acid, nitric, or phosphoric acid, a stabilizing agent, and balances with demineralized water as an ingredient.

[0069] The composition of the present invention includes hydrogen peroxide from about 2-40 percent, preferably 2 to 20 percent, and more preferably, 2 to 8 percent.

[0070] The composition of the present invention includes glacial acetic acid from about 40 to 90 percent, preferably 60 to 80 percent, and more preferably from 70 to 80 percent.

[0071] The composition of the present invention includes stabilizing agent compounds like EDTA, HEDP, 2,6-pyridine dicarboxylic acid, and other proper stabilizers are used in the amount of 0.1 to 10 percent, preferably 0.2 to 5 percent and more preferably with 0.5 to 1.5 percent.

[0072] The composition of the present invention includes mineral acid compounds like nitric acid and phosphoric acid from about 1 to 30 percent, preferably 5 to 20 percent, and more preferably with 7 to 10 percent.

[0073] Preparation of the formulations:

[0074] 4 different solutions in Table 2 were synthesized by combining the mentioned percentages. The molar ratio of hydrogen peroxide and acetic acid in these formulations is considered so that the concentration of peracetic acid in the final solution is about 4 and 8.

[0075] To better compare the formulations made in this present invention in terms of performance, 4 comparative solutions with similar formulations in the final product commercially in Table 1 were prepared with the percentage of raw material compositions according to Table 3.

[0076] For the acid-sanitizers solutions to reach equilibrium, after ten days, the percentage of peroxyacetic acid formed and hydrogen peroxide was measured using oxidation-reduction titration and iodometry methods, which is shown in Table 4.

[0077] Stability test:

[0078] To measure the stability of the product, the prepared solutions were kept at 25℃, and over time, using oxidation-reduction titration and iodometry, the amount of hydrogen peroxide and peracetic acid was measured. The results are shown in table 5.

[0079] Examining the numbers in the above table shows that all the solutions made in the time range of 6 months have good stability and no appreciable amount of peracetic acid and hydrogen peroxide was observed during the time.

[0080] As can be seen from the above table, all the solutions made in the time range of 6 months have good stability, and no significant reduction of peracetic acid and hydrogen peroxide was observed over time.

[0081] Antimicrobial test:

[0082] Analyzing the minimum inhibitory concentration (MIC) shows the lowest concentration of an antimicrobial product that prevents visible growth of the desired microorganism, under the test conditions. In this method, the samples are diluted with a concentration of 200 ppm in standard hard water. The test sample was diluted with a difference of 10 ppm using a TSB culture medium. After preparing the samples, one milliliter of prepared microbial suspension (half McFarland's) was added to all the tubes and incubated for 24 hours at 35°C. After the end of the incubation time, the tubes were checked for turbidity and the first tube with no turbidity was considered as the MIC concentration.

[0083] Tubes in which no turbidity was observed were cultured linearly on TSA medium and incubated again at 35°C for 24 hours. After the mentioned time, the tubes were checked for microorganism growth and the concentration of the tube without growth was considered as minimum bactericidal concentration (MBC).

[0084] To measure and compare the antimicrobial potential of the prepared solutions, the MIC and MBC values of the solutions were measured on 2 microbial strains of E.Coli (ATCC 10536) and Candida Albicans (ATCC 10231), and the result is shown in tables 6 to 8.

[0085] As can be seen from Table 8, the MIC and MBC values of the prepared solutions are slightly higher than the comparative solutions, but all the solutions are effective at a concentration of less than 150 ppm according to the effective ingredient peracetic acid suggested by the FDA.

[0086] Power of dissolution test:

[0087] Considering that the prepared solutions are used as acid-sanitizer products, in addition to their antimicrobial ability, they should also be able to dissolve mineral scale. Since the mineral deposits that exist in the production lines of the dairy and food industries generally include mostly calcium phosphate, calcium carbonate, and magnesium carbonate, these three salts are used to compare the descaling power of the mineral deposits of the prepared solutions.

[0088] First, according to the percentage of peracetic acid in each of the acid-sanitizer solutions synthesized in Table 1, formulations 1,2 and comp 1,2 at a ratio of 1:400, and formulations 3,4 and comp 3,4 at a ratio of 1: 200 were diluted with distilled water so that the final concentration of peracetic acid in the final diluted solutions is about 200 ppm.

[0089] To analyze the descaling potential of the solutions, three kinds of mineral salt powder have been prepared and tested. For this aim, 1.5 grams of the mineral salt was weighed and poured into a 250 Erlenmeyer. Then, 50 grams of the acid-sanitizer with the mentioned concentration was added to it.

[0090] A magnetic stirrer with a speed of 100 rpm was used to create turbulence in the Erlenmeyer containing mineral salt powder and diluted acid-sanitizer solution. The duration of this process for each test was 5 minutes and the temperature was stable during the whole process and was set at 25 centigrade degrees.

[0091] After the mentioned time, the solutions are passed through Watson 42 filter paper to separate the remaining and undissolved mineral salt powder. Then, the remaining mineral salt powder was washed using 50 cc of distilled water in 3 steps. At the end, the filter paper containing the remaining mineral salts was placed in a 40 ℃ oven for 24 hours, and then the weight of the remaining mineral salt was measured. The results are shown in Tables 9 to 11. Also, the dissolved percentage of each of the mineral salts in the acid-sanitizer solution is shown in Table 12 in compared form.

[0092] Examining the results in Table 8 shows that the solutions made based on the formula of this patent (Example 1 to 4) have more dissolving power of all three mineral deposits of calcium phosphate, calcium carbonate, and magnesium carbonate compared to similar formulas (comparative solutions 1 to 4). This is even though in the formulas that are compared with each other, such as the formula of Example 1 with comp 1, the type and amount of nitric acid in the concentrated and ready-to-use solution are the same. This comparison also applies to the formula of example 2 and com 2, which have the same amount of phosphoric acid. In general, the solutions made in this patent, while having appropriate antimicrobial properties, have much better de-scaling power than the commercial solutions available in the market and the formulations of other patents with similar compounds.

[0093] To sum up, the invention reduces the six steps of the traditional CIP operation, into 4 steps.

[0094] The six traditional steps are rinse, alkaline cleaning, intermediate rinse, acid cleaning, final rinse, disinfection

[0095] This invention eliminates the last four steps and does it all in one single step.Advantage effects of the invention

[0096] Peracetic acid has many advantages over other disinfectant compounds.

[0097] Broad spectrum antimicrobial,

[0098] no dangerous residue,

[0099] high oxidizing power,

[0100] bleaching properties,

[0101] cost-effective

[0102] very widely used products in food, dairy, beverage, agriculture, water treatment, oil and gas, pulp & paper, medicine, and dentistry industries.

[0103] Decrease step of the CIP process from 6 into 4 steps

[0104] Reducing energy consumption ( water and electricity)Examples

[0105] [Table 1]: formulations of available acid-sanitizing compositions which are produced commercially

[0106] [Table. 2]: Acid-sanitizer formulations of the present invention

[0107] [Table. 3]: formulations of comparative examples:

[0108] [Table. 4]: weight percentage of the main component of samples

[0109] [Table. 5]: long term stability evaluation of samples according to concentration of hydrogen peroxide and peracetic acid

[0110] [Table. 6]: the result of MIC and MBC of E.Coli (ATCC 10536)

[0111] [Table. 7]: Result of MIC and MBC of Candida Albicans (ATCC 10231)

[0112] [Table. 8]: the MIC and MBC values of the prepared solutions briefly

[0113] [chart. 1]: The amount of calcium carbonate dissolution in different samples

[0114] [chart. 2]: The amount of magnesium carbonate dissolution in different samples

[0115]

[0116] [chart. 3]: The amount of calcium phosphate dissolution in different samples

[0117] [Table. 9]: The percentage of dissolution of mineral salts in different samples

[0118] Peracetic acid has a strong, pungent, vinegar-like odor that hurts the human mucus and it has a high oxidizing power its touch with the body's skin is dangerous and it must be used with caution and by the use of safety equipment. It can also be used in different industries like agriculture, dentistry, dairy, oil and petrol industry, paper industry, etc. Furthermore, it is used for COP (Cleaning on place) and CIP (cleaning in place)

Claims

A composition comprises of Peracetic acid, Nitric acid, Acetic acid (glacial), Hydrogen peroxide, Phosphoric acid, HEDP as a stabilizer, and deionized waterAccording to the claim. 2, the descaling power of the composition depends directly on the amount of Acetic and nitric acid in itAccording to the claim. 2, the nitric acid in the formulation helps descaling and disinfection to happen simultaneouslyAccording to the claim. 3, the simultaneous sanitation and descaling reduce the CIP stagesAccording to the claim. 4, for the CIP stages to be less, the composition contains safe raw materials, therefore no rinsing is needed in the final stage

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