Chlorine-containing foam disinfection effervescent tablet and preparation method thereof

Abstract

The invention provides a chlorine-containing foam disinfection effervescent tablet and a preparation method thereof, and belongs to the technical field of veterinary disinfectants. The foam disinfection effervescent tablet is prepared from the following components: a chlorine-containing disinfectant, a composite surfactant, an effervescing agent, a stabilizer, an adhesive and a filler, the foam disinfection effervescent tablet comprises the following components in percentage by mass: 10-40% of a chlorine-containing disinfectant, 10-50% of a composite surfactant, 5-30% of an effervescing agent, 0-10% of a stabilizer, 0-5% of an adhesive and the balance of a filler. The foam disinfection effervescent tablet is convenient to use, can be rapidly dissolved in water, can form stable foam, improves the visibility and vertical surface adhesiveness of disinfection coverage, ensures that available chlorine keeps high activity at a proper pH value, is good in stability of the available chlorine, is convenient to transport and store, is simple in preparation process, is controllable in cost, and is suitable for industrial production. The disinfection requirements of large-scale breeding scenes such as pastures are met.

Description

Technical Field

[0001] This invention belongs to the field of disinfectant technology, specifically relating to a chlorine-containing foam disinfectant effervescent tablet and its preparation method. Background Technology

[0002] Currently, the main disinfectants used in livestock farms include chlorine-containing disinfectants (such as potassium persulfate compound salt, sodium dichloroisocyanurate, trichloroisocyanuric acid, hypochlorous acid, etc.), caustic soda, acidifying agents, glutaraldehyde and its compounds, etc. With the introduction of African swine fever virus into livestock farming in my country at the end of 2018, the use of veterinary disinfectants in my country experienced explosive growth (62.7%) in 2018-2019, and is expected to continue growing at a rate of nearly 10% from 2019 to 2022. To date, the use of chemical disinfectants remains the primary means of preventing various pathogens and viruses in livestock farming, and is the first choice for biosecurity control.

[0003] Chlorine-based disinfectants are widely used in ranches due to their low price, broad sterilization spectrum, low dosage, and good disinfection effect. They are primarily used by spraying and soaking. However, traditional common chlorine-based disinfectants (such as sodium dichloroisocyanurate powder) have many insurmountable technical defects in actual ranch use, severely limiting disinfection effectiveness and user experience, as follows:

[0004] First, the lack of visibility in disinfection coverage can easily create loopholes in defense.

[0005] The ranch contains many dark areas (such as corners of livestock sheds, feed storage rooms, and inside ventilation ducts). Ordinary chlorine-based disinfectants, once dissolved, are transparent liquids, making it difficult to visually determine the sprayed area and coverage after spraying. Operators cannot visually identify "unsprayed areas" or "unevenly covered areas," easily creating disinfection blind spots. This leads to pathogen residues, creating a hidden danger for disease transmission and seriously affecting the integrity of the ranch's disease prevention efforts.

[0006] Second, the vertical disinfection process suffers from insufficient adhesion and inadequate disinfection time.

[0007] Ranches have numerous vertical structures (such as livestock shed walls, metal pens, and water / sewage pipes). Due to surface tension and gravity, ordinary chlorine-based disinfectants quickly slide off vertical surfaces after spraying, failing to maintain sufficient contact time. While most chlorine-based disinfectants require 3-5 minutes of contact with pathogens to achieve optimal disinfection, ordinary liquid disinfectants often remain on vertical surfaces for less than 1 minute, resulting in insufficient disinfection and inability to completely kill pathogens.

[0008] 3. In complex environments, "weak permeability" leads to incomplete cleaning and disinfection.

[0009] Pasture environments are complex, containing pollutants such as fecal residue, feed debris, and biofilm. Furthermore, structures like pens and pipes often have gaps and folds (such as welded seams in pens and folds in the inner walls of pipes). Ordinary chlorine-based disinfectants have weak penetrability and struggle to penetrate the physical barriers of pollutants or reach the intricate details of complex structures. This results in ineffective cleaning of pollutants and incomplete disinfection of pathogens hidden within, thus compromising the effectiveness of disease prevention.

[0010] To address these issues, targeted solutions have emerged in related technical fields. For example, patent CN202110188804.9 discloses a chlorine-containing alkaline foam cleaning agent that extends the adhesion time of the disinfectant to the stain surface through foam, achieving integrated cleaning and disinfection. However, this cleaning agent is an alkaline system (product pH ≥ 13.0), which reduces the oxidizing power of the chlorine-containing disinfectant, resulting in a significantly lower disinfection effect compared to acidic systems. Furthermore, as a liquid product, this cleaning agent incurs high transportation costs over long distances, and the effective chlorine in the liquid system has poor stability, making it prone to decomposition due to changes in the storage environment, affecting the product's shelf life and effectiveness.

[0011] To address the transportation and stability issues of liquid chlorine-based disinfectants, another patented technology (CN202411372784.0) proposes a powdered foam organochlorine disinfectant. This technology improves the stability of available chlorine through the adsorption and encapsulation of organochlorine by modified magnesium sulfate and the synergistic effect of sodium dimethylbenzenesulfonate and surfactants. However, this technology uses a powder formulation, making it difficult for operators to use in precise quantities. Furthermore, the chlorine-containing powder is easily dispersed, irritating and affecting personnel health. The complexity and cost of this process also limit its widespread application in ranch settings. Firstly, modified magnesium sulfate requires multiple complex processes including ball milling, polysilicic acid preparation, ultrasonic stirring, and centrifugal drying. The adsorption / encapsulation process of organochlorine and surfactants requires extremely high control of process parameters, and operational deviations can easily lead to uneven adsorption and insufficient encapsulation coverage, thus affecting the stable release of available chlorine. Secondly, the complex preparation process not only increases investment in production equipment but also extends the production cycle, significantly increasing product conversion costs. This contradicts the actual needs of farms to reduce costs and increase efficiency, making large-scale widespread application difficult.

[0012] In summary, existing chlorine-based foam disinfectant technologies either suffer from reduced disinfection effectiveness due to unsuitable system pH, high transportation costs due to liquid form, or are difficult to adapt to ranch scenarios due to complex processes, high costs, unstable adsorption and encapsulation effects, and inconvenience in use. There is an urgent need to develop a chlorine-based disinfection technology that combines excellent disinfection effect, stable available chlorine, convenient transportation and storage, simple process, and controllable cost to meet the actual application needs of large-scale livestock farming. Summary of the Invention

[0013] The purpose of this invention is to overcome the defects of the existing technology and provide a chlorine-containing foam disinfectant effervescent tablet and its preparation method.

[0014] To achieve the above objectives, the present invention adopts the following technical solution:

[0015] In a first aspect, the present invention provides a chlorine-containing foam disinfectant effervescent tablet, the foam disinfectant effervescent tablet comprising the following components: a chlorine-containing disinfectant, a composite surfactant, an effervescent agent, a stabilizer, a binder, and a filler.

[0016] The components and their mass percentages in the foam disinfectant effervescent tablets are as follows: 10-40% chlorine-containing disinfectant, 10-50% compound surfactant, 5-30% effervescent agent, 0-10% stabilizer, 0-5% binder, and the remainder is filler.

[0017] Preferably, the components and their mass percentages in the foam disinfectant effervescent tablets are as follows: 20-40% chlorine-containing disinfectant, 15-40% compound surfactant, 10-30% effervescent agent, 3-10% stabilizer, 0.5-3% binder, and the remainder is filler.

[0018] More preferably, the components and their mass percentages in the foam disinfectant effervescent tablets are as follows: 20-40% chlorine-containing disinfectant, 20-40% compound surfactant, 10-30% effervescent agent, 3-10% stabilizer, 0.5-3% binder, and the remainder is filler.

[0019] The chlorine-containing disinfectant is selected from one or more of sodium dichloroisocyanurate, trichloroisocyanuric acid, and calcium hypochlorite.

[0020] Preferably, the chlorine-containing disinfectant is selected from sodium dichloroisocyanurate and trichloroisocyanuric acid, and more preferably sodium dichloroisocyanurate.

[0021] The composite surfactant is selected from one or more of sodium dodecyl sulfate, sodium fatty acid methyl ester sulfonate, sodium dodecyl sulfonate, sodium dodecylbenzene sulfonate, sodium α-alkenyl sulfonate, sodium cocoyl glutamate, sodium cocoyl hydroxyethyl sulfonate, and sodium lauroyl sarcosinate.

[0022] Preferably, the composite surfactant is a combination of sodium dodecylbenzene sulfonate, sodium fatty acid methyl ester sulfonate, and sodium cocoyl hydroxyethyl sulfonate.

[0023] Preferably, the mass ratio of sodium dodecylbenzenesulfonate, sodium fatty acid methyl ester sulfonate, and sodium coconut oil hydroxyethyl sulfonate in the composite surfactant is (1-4):(1-4):(0.2-2); more preferably, the mass ratio is 2:2:1.

[0024] The effervescent agent contains both an alkaline source and an acidic source.

[0025] Preferably, the alkaline source in the effervescent agent is selected from one or both of sodium bicarbonate and sodium carbonate.

[0026] More preferably, the alkaline source in the effervescent agent is sodium bicarbonate.

[0027] Preferably, the acid source in the effervescent agent is selected from one or more of malic acid, anhydrous citric acid, sodium bisulfate, boric acid, fumaric acid, adipic acid, cyanuric acid, and aminosulfonic acid.

[0028] More preferably, the acid source in the effervescent agent is anhydrous citric acid or aminosulfonic acid.

[0029] The stabilizer is selected from one or more of sodium tripolyphosphate, sodium pyrophosphate, tetrasodium hydroxyethylidene diphosphonate, aminotrimethylphosphonic acid, 2-hydroxyphosphonoacetic acid, sodium hexametaphosphate, and disodium EDTA.

[0030] Preferably, the stabilizer is selected from sodium hexametaphosphate and tetrasodium hydroxyethylidene diphosphonate.

[0031] The adhesive is selected from one or more of sodium carboxymethyl cellulose, xanthan gum, carrageenan, hydroxyethyl cellulose, and polyethylene glycol.

[0032] Preferably, the adhesive is selected from xanthan gum and polyethylene glycol (molecular weight ≥ 4000).

[0033] The filler is selected from one or more of anhydrous glucose, sucrose, lactose, maltodextrin, anhydrous sodium sulfate, and sodium chloride.

[0034] A preferred formulation of chlorine-containing foam disinfectant effervescent tablets is as follows: the components and their mass percentages in the foam disinfectant effervescent tablets are: sodium dichloroisocyanurate 30-40%, composite surfactant 25-40%, sodium bicarbonate 5-15%, anhydrous citric acid 3-8%, aminosulfonic acid 2-5%, tetrasodium hydroxyethylidene diphosphonate 0.5-1%, sodium hexametaphosphate 4-8%, xanthan gum 0.2-1%, polyethylene glycol 0.5-2%, and the balance being lactose; the composite surfactant is composed of sodium dodecylbenzenesulfonate, sodium fatty acid methyl ester sulfonate, and sodium cocoyl hydroxyethyl sulfonate in a mass ratio of 2:2:1.

[0035] In a second aspect, the present invention provides a method for preparing chlorine-containing foam disinfectant effervescent tablets, the steps of which are as follows:

[0036] Step S2-1: Pass the effervescent agent, stabilizer, binder, and filler through a 20-mesh sieve respectively;

[0037] Step S2-2: Weigh out the surfactant, effervescent alkali source, part of the binder and filler according to the formula and add them to the mixing equipment. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system A;

[0038] Step S2-3: Weigh out the chlorine-containing disinfectant, effervescent acid source, stabilizer, and remaining binder according to the formula and add them to the mixing equipment of powder system A. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system B.

[0039] Step S2-4: Powder system B is granulated using a dry granulation method. The prepared granules are then compressed into tablets using a rotary tablet press, with a tablet weight of 1.0-5.0g, thus obtaining chlorine-containing foam disinfectant effervescent tablets.

[0040] The method of using the chlorine-containing foam disinfectant effervescent tablets of this invention is as follows:

[0041] Method 1: Dissolve the disinfectant effervescent tablets in tap water at a mass ratio of 1:20 to obtain a disinfectant concentrate. Place the concentrate in a spray gun with a foaming nozzle and use a high-pressure cleaning device to adjust the disinfectant concentrate to a water ratio of 1:10 to 1:25. Spray the disinfectant concentrate onto the surface of the object to be disinfected. The diluted disinfectant solution forms foam on the surface of the object and adheres to it.

[0042] Method 2: Dissolve the disinfectant effervescent tablets in tap water at a mass ratio of 1:200 to 1:500 to obtain a disinfectant dilution. Use a high-pressure cleaning device with a foaming nozzle to spray the disinfectant dilution onto the surface of the object to be disinfected. The disinfectant dilution forms foam on the surface of the object and adheres to the surface.

[0043] Both the disinfectant concentrate and the disinfectant dilution are weakly acidic (pH 5.5-7.0). This weakly acidic system helps maintain the stability of chlorine in the solution, effectively inhibiting its hydrolysis and promoting the stable presence of available chlorine components. This ensures the chemical stability, long-lasting effect, and safety of the product.

[0044] This invention selects Staphylococcus aureus (ATCC 6538) and Escherichia coli (8099) as indicator microorganisms to study the disinfection effect of these indicator bacteria on environmental surfaces. It also selects a poliovirus type 1 (PV-I) vaccine strain as an indicator virus to study its disinfection effect against the virus. Experimental results show that the formulation of this invention meets national disinfection standards for environmental surface disinfection and is superior to sodium dichloroisocyanurate solution with the same effective chlorine concentration, making it widely applicable for disinfection in livestock farms.

[0045] The present invention has the following beneficial effects:

[0046] 1. Excellent foam stability, enhancing disinfection visibility and adhesion: Through the selection of superior composite surfactants, stable and abundant foam can be formed in aqueous solutions. The foam clearly shows the disinfection coverage area, avoiding blind spots; at the same time, the viscosity and retention of the foam allow the disinfectant to adhere to vertical structures (such as walls and pipes) for a long time, ensuring that the disinfection time meets the standard (retention time ≥ 5 minutes) and improving the disinfection effect.

[0047] 2. High stability of available chlorine and long shelf life: The stabilizer used can inhibit the decomposition of chlorine-containing disinfectants by chelating metal ions and regulating the microenvironment of the system. Furthermore, the tablet form avoids the instability caused by hydrolysis and oxidation of available chlorine in liquid systems, and also avoids the effects of stratification due to the high water absorption and different particle sizes of powders. After being stored at 37℃~40℃ for 3 months, the available chlorine retention rate remains ≥95%, meeting the stability test requirements of disinfection products in Section 2.2.3 of the "Disinfection Technical Specifications" (2002 edition). The shelf life is set at 2 years.

[0048] 3. Convenient transportation, storage, and use, resulting in reduced costs: Compared to powder and liquid foam disinfectants, tablets are easier to use and dispense in measured quantities, eliminating dust spillage and the irritation and harm to humans caused by chlorine-containing disinfectants; during transportation, there is no need to consider leakage prevention or reduce transportation weight (with the same effective ingredients, the volume is smaller and the weight is lighter), significantly reducing transportation costs; at the same time, the storage conditions for tablets are easier to meet (no need for strict temperature control, anti-freezing, etc.), and storage costs are also significantly reduced.

[0049] 4. Compared to regular tablets, effervescent tablets can rapidly disintegrate into a uniform solution within 5 minutes of dissolving in water. This avoids problems such as excessively high concentrations and drastic pH changes during localized dissolution of regular tablets, which can lead to decreased stability of chlorine-containing disinfectants.

[0050] 5. Simple preparation process, suitable for ranch needs: The preparation process only requires simple steps such as mixing and sieving, without the need for complex adsorption, encapsulation or modification processes. The production equipment investment is small, the cycle is short, and the conversion cost is low, which can meet the needs of large-scale breeding scenarios such as ranches for low-cost and easy-to-operate disinfection products.

[0051] 6. Excellent disinfection effect and strong adaptability: The components selected in this invention are all highly water-soluble, and they dissolve rapidly in synergy with the composite surfactant. After the chlorine-containing foam disinfectant dissolves in water, the system can maintain a weakly acidic environment of pH 5.5-7.0 through the synergistic effect of each component, resulting in a high proportion of hypochlorous acid molecules and strong disinfection activity. After being stored at room temperature for 72 hours after dissolution, the effective chlorine retention rate is still ≥90%. At the same time, the permeability of the foam helps the disinfectant penetrate the pollutant barrier and reach deep into the gaps of complex structures, improving the disinfection effect in complex environments. Attached Figure Description

[0052] Figure 1 Chlorine-containing foam disinfectant effervescent tablets;

[0053] Figure 2 Schematic diagram of foam adhesion in embodiment 4 of the present invention. Detailed Implementation

[0054] The above content will be further described in detail below through specific embodiments. However, this should not be construed as limiting the scope of the above subject matter to the following embodiments. All technologies implemented based on the content of this invention fall within the scope.

[0055] Examples 1-8: A Chlorine-Containing Foam Disinfectant Effervescent Tablet

[0056] Table 1. Formulations (g) of chlorine-containing foam disinfectant effervescent tablets in Examples 1-8 of the present invention.

[0057]

[0058] The preparation method of the chlorine-containing foam disinfectant effervescent tablets includes the following steps:

[0059] Step S2-1: Pass sodium bicarbonate, anhydrous citric acid, aminosulfonic acid, tetrasodium hydroxyethylidene diphosphonate, sodium hexametaphosphate, polyethylene glycol, and lactose through a 20-mesh sieve (filter immediately before use);

[0060] Step S2-2: Weigh out sodium dodecylbenzenesulfonate, sodium fatty acid methyl ester sulfonate, sodium cocoyl hydroxyethyl sulfonate, sodium bicarbonate, xanthan gum, and lactose according to the above prescription and add them to the mixing equipment. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system A.

[0061] Step S2-3: Weigh out sodium dichloroisocyanurate, anhydrous citric acid, aminosulfonic acid, tetrasodium hydroxyethylidene diphosphonate, sodium hexametaphosphate, and polyethylene glycol according to the above prescription and add them to the mixing equipment of powder system A. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system B.

[0062] Step S2-4: Powder system B is granulated using a dry granulation method. The prepared granules are then compressed into tablets using a rotary tablet press, with a tablet weight of 1.0-5.0g, thus obtaining chlorine-containing foam disinfectant tablets.

[0063] In Comparative Example 1, the composite surfactant formulation in Example 4 was replaced with 17.5g each of sodium α-olefin sulfonate and sodium dodecyl sulfate, while other components, dosages, and preparation methods remained unchanged.

[0064] Comparative Example 2 removed the effervescent agent from Example 4, while keeping other components, dosages, and preparation methods unchanged, and added lactose to 100g to prepare foam disinfectant tablets.

[0065] In Comparative Example 3, the stabilizer formulation in Example 4 was replaced with 0.5g of sodium pyrophosphate and 5g of disodium EDTA, while other components, dosages, and preparation methods remained unchanged.

[0066] Test Example 1: Tablet Property Detection Test

[0067] 1. Tablet forming test

[0068] (1) Tablet hardness and molding test

[0069] Using a tablet hardness tester, the tablet hardness should be ≥50N, indicating good tablet formation, no cracks or burrs; otherwise, it is unqualified. The results are shown in Table 2.

[0070] (2) Tablet solubility test

[0071] The dissolution rate and solubility were verified using high hard water dissolution rate and solubility tests.

[0072] Examples 1-8 and Comparative Examples 1-2 were mixed with high-hardness water (500 mg / L of calcium carbonate) at a mass ratio of 1:200, left to stand in an open container, and the time for complete dissolution was recorded as <5 min. After standing for 30 min, it was observed that the solution should be completely dissolved and clear; otherwise, it was considered unqualified. The results are shown in Table 2.

[0073] 2. Foam adhesion and foaming power test

[0074] (1) Foam Adhesion Test

[0075] The above Examples 3-8 and Comparative Examples 1-3 were prepared by mixing tap water at a mass ratio of 1:500 to prepare disinfectant dilutions. The disinfectant dilutions were sprayed onto the surface of the object to be disinfected using a high-pressure cleaning device with a foaming nozzle. The disinfectant dilutions formed foam on the surface of the object and adhered to the vertically placed clean glass surface. The foam adhesion time was recorded. An adhesion time of ≥5 minutes was considered qualified, otherwise it was unqualified. The results are shown in Table 3.

[0076] (2) Foaming power test

[0077] According to GB / T 7462-94 "Determination of Foaming Power of Surfactants - Modified Ross-Miles Method", the foaming power for 30 seconds and 5 minutes was determined. The foaming power for 30 seconds was ≥280 mm, and the foaming power for 5 minutes was ≥220 mm. Otherwise, it was considered unqualified. The results are shown in Table 3.

[0078] 3. Stability test

[0079] (1) Detection of the decrease rate of effective chlorine in tablets after 3 months

[0080] The initial available chlorine content W0 and the available chlorine content W1 after 3 months of storage at 37℃~40℃ were determined according to the method in section 2.2.1.2.1 of the 2002 edition of the "Disinfection Technical Specifications". The available chlorine reduction rate was calculated using the formula (W1-W0) / W0*100%. If the available chlorine reduction rate of dry powder exceeds 10%, the tablet stability is unqualified, and vice versa. The results are shown in Table 3.

[0081] (2) Detection of the decrease rate of available chlorine in the solution after 72 hours

[0082] Examples 3-8 and Comparative Examples 1-3 were prepared by mixing tap water at a mass ratio of 1:200 to form disinfectant dilutions, which were then stored indoors in an open environment for 72 hours. The available chlorine content (W2) and W3 at 0 hours and 72 hours were determined according to method 2.2.1.2.1 of the 2002 edition of the "Disinfection Technical Specifications". The available chlorine reduction rate was calculated using the formula (W3-W2) / W2*100%. If the available chlorine reduction rate exceeded 5%, the solution was deemed to have unqualified stability in water; otherwise, the stability in water was deemed qualified. The results are shown in Table 3.

[0083] Table 2. Stability testing of chlorine-containing foam disinfectant tablets in the embodiments of the present invention.

[0084] Formula Example 1 Example 2 Example 3 Example 4 Example 5 Tablet hardness 25N 70N 97N 104N 170N Tablet forming Fragmentation Molding is generally Well formed Well formed Well formed Dissolution rate / / / 2 minutes 30 seconds 4 minutes and 55 seconds High hard water solubility / turbid turbid clarify clarify in conclusion Unqualified Unqualified Unqualified qualified qualified Formula Example 6 Example 7 Example 8 Comparative Example 1 Comparative Example 2 Tablet hardness 162N 128N 85N 95N 270N Tablet forming Well formed Well formed Well formed Well formed excellent Dissolution rate 4 minutes 00 seconds 3 minutes and 10 seconds 4 minutes and 40 seconds 3min55s 20min05s High hard water solubility clarify clarify clarify turbid clarify in conclusion qualified qualified qualified Unqualified Unqualified

[0085] Table 3. Foaming and stability tests of chlorine-containing foam disinfectant tablets in the embodiments of the present invention.

[0086]

[0087]

[0088] Experimental results show that the amount of different composite surfactants added is the main factor affecting foam, tablet hardness and dissolution rate.

[0089] Example 1: High effervescent agent content, no stabilizer or binder added; tablets easily cracked and failed to form. Example 2: Based on Example 1, a binder was added; tablet formation was average, and the solution was cloudy when dissolved in hard water. Example 3: Based on Example 2, the effervescent agent was optimized; tablet formation was good, but the solution was cloudy and unacceptable when dissolved in hard water. Example 4: Based on Example 3, a stabilizer was added; the tablets dissolved quickly in hard water, and the solution was clear and transparent, indicating that the optimized effervescent agent, stabilizer, and binder all played a stabilizing role in the chlorine-containing foam disinfectant effervescent tablets of this invention.

[0090] Examples 4, 6, 7, and 8 benefited from their stability; the tablets and solutions exhibited satisfactory effective chlorine stability, with dissolution times in hard water all < 5 minutes and foam adhesion times > 5 minutes. Examples 4 and 8 showed the best foaming power and foam adhesion time. Example 4 had the fastest hard water dissolution rate. Example 5 showed the best effective chlorine stability in both tablets and solutions, but its foaming power was low and its foam adhesion time was short. Considering cost, quality testing, stability, and foam adhesion effect, the product of Example 4 was the best.

[0091] The results of Example 4 compared with Comparative Example 1 show that the composite surfactant added in Example 4 has better stability against other composite surfactants, does not affect the effective chlorine stability, and has better hard water resistance.

[0092] The results of Example 4 compared with Comparative Example 2 show that the effervescent agent added in Example 4 helps with tablet formation, facilitates rapid dissolution in water, and improves ease of use.

[0093] The results of Example 4, compared with Comparative Example 3, show that the stabilizer added in Example 4 has a better effect on the stability and water-soluble stability of the tablets of the present invention. In Comparative Example 3, the stabilizing components were destroyed by the high-chlorine oxidant, affecting the effectiveness of the stabilizer.

[0094] The following experimental examples compare the disinfection effects of Examples 4, 6, 7, and 8 with the control group (commercially available 20% sodium dichloroisocyanurate powder) and Comparative Example 1. The Staphylococcus aureus (ATCC 6538) and Escherichia coli (8099) used were obtained from the China General Microbiological Culture Collection Center, and the poliovirus type 1 (PV-I) vaccine strain was obtained from the Institute of Virology, Chinese Center for Disease Control and Prevention.

[0095] Experiment Example 2: Chlorine-containing foam disinfection effervescent tablet sterilization experiment

[0096] 1. Reagents and Equipment

[0097] (1) Strains: Staphylococcus aureus ATCC 6538, Escherichia coli 8099.

[0098] (2) Disinfectants for the control group, comparative example 1, examples 4, 6, 7 and 8 were prepared using sterile hard water according to the available chlorine concentration. The prepared concentration was 1.25 times the concentration to be tested. They were then placed in a water bath at 20℃±1℃ for later use.

[0099] (3) Neutralizing agent: D / E neutralizes broth.

[0100] (4) Diluent: Tryptone saline solution (TPS).

[0101] (5) Culture medium: Tryptone soybean agar medium (TSA).

[0102] (6) Organic interfering substance: bovine serum albumin.

[0103] 2. Methods (The tests were conducted according to Section 2.1.1.7.4 of the "Disinfection Technical Specifications" (2002 edition) and Section 5.4.5 of GB / T 38502-2020 "Laboratory Test Methods for the Sterilization Efficacy of Disinfectants").

[0104] (1) The disinfectants of the control group, comparative example 1, examples 4, 6, 7 and 8 were prepared with an effective chlorine concentration of 200 mg / L. The neutralizing agent identification test was carried out. The test was repeated three times.

[0105] (2) The prepared 1.25 times concentration disinfectant solution was mixed with Staphylococcus aureus and Escherichia coli suspensions containing organic interfering substances according to the method (8:2). The reaction times were 5 min, 10 min, and 15 min, with effective chlorine concentrations of 200 mg / L, 100 mg / L, and 50 mg / L, respectively. After the reaction time was completed, a neutralizing agent was added to stop the reaction. At the same time, a diluent was used instead of disinfectant solution to conduct parallel tests as a positive control. The test was repeated three times.

[0106] (3) All test samples were cultured in an incubator at 37℃ for 48 hours. The concentration of viable bacteria was counted and converted to logarithmic values ​​to calculate the kill logarithmic value.

[0107] 3. Regulations for the Evaluation of Bactericidal Tests

[0108] If the kill log value is ≥5.00 for each test, the disinfection is considered qualified; otherwise, it is considered unqualified.

[0109] 4. Results

[0110] (1) Chlorine-containing disinfectants were prepared using products from the control group, comparative example 1, and examples 4, 6, 7, and 8. D / E neutralizing broth can effectively neutralize the effect of the disinfectant on Staphylococcus aureus and Escherichia coli in the mixture. Furthermore, the neutralizing agent and neutralization product have no adverse effects on Staphylococcus aureus, Escherichia coli, and the culture medium, indicating that the neutralizing agent is qualified.

[0111] (2) When the effective chlorine concentration of the chlorine-containing disinfectant in the control group was 50 mg / L, the average log killing value of Staphylococcus aureus and Escherichia coli after 5 min and 10 min was <5.00, and the disinfection effect was unqualified; after 15 min, the average log killing value of Staphylococcus aureus and Escherichia coli was >5.00, and the disinfection effect was qualified.

[0112] (3) In Examples 4, 6, 7, and 8, when preparing chlorine-containing disinfectant solutions with an effective chlorine concentration of 50 mg / L, the average log reduction values ​​against Staphylococcus aureus and Escherichia coli were all <5.00 after 5 minutes of exposure, indicating that the disinfection effect was unqualified. After 10 minutes and 15 minutes of exposure, the average log reduction values ​​against Staphylococcus aureus and Escherichia coli were >5.00, indicating that the disinfection effect was qualified.

[0113] (4) The chlorine-containing disinfectant solutions prepared in the control group and Examples 4, 6, 7 and 8 had effective chlorine concentrations of 200 mg / L and 100 mg / L, respectively. After acting for 5 min, 10 min and 15 min, respectively, the average log killing value of Staphylococcus aureus and Escherichia coli was >5.00, and the disinfection effect was qualified.

[0114] (5) When the effective chlorine concentration of the chlorine-containing disinfectant in Comparative Example 1 was 200 mg / L, the average log kill value against Staphylococcus aureus and Escherichia coli was <5.00 after 5 min of action, and the disinfection effect was unqualified; the average log kill value against Staphylococcus aureus and Escherichia coli was >5.00 after 10 min and 15 min of action, and the disinfection effect was qualified; when the effective chlorine concentration was 50 mg / L and 100 mg / L, the average log kill value against Staphylococcus aureus and Escherichia coli was <5.00 after 5 min, 10 min and 15 min of action, respectively, and the disinfection effect was unqualified.

[0115] 5. Conclusion

[0116] The chlorine-containing disinfectant solutions prepared in Examples 4, 6, 7, and 8 showed better killing effects against Staphylococcus aureus and Escherichia coli than the chlorine-containing disinfectant used in the control group, and were significantly better than Comparative Example 1 (see Table 4).

[0117] Table 4. Killing effect of disinfectant solutions of different concentrations on Staphylococcus aureus and Escherichia coli.

[0118]

[0119] Test Example 3: Virus Inactivation Test of Chlorine-Containing Foam Disinfectant Tablets

[0120] 1. Reagents and Equipment

[0121] (1) Experimental virus strain: poliovirus type I (PV-I) vaccine strain.

[0122] (2) BGM cells.

[0123] (3) Using the control group, comparative example 1, examples 4, 6, 7 and 8, the effective chlorine was calculated and prepared using sterile hard water. The concentration of the prepared solution was 1.25 times that of the concentration to be tested, and it was placed in a water bath at 20℃±1℃ for later use.

[0124] (4) Neutralizing agent: D / E neutralizes broth.

[0125] (5) Cell maintenance culture medium.

[0126] (6) Complete cell culture medium.

[0127] (7) Organic interfering substance: bovine serum albumin.

[0128] (8) 96-well culture plate.

[0129] (9) Inverted microscope.

[0130] 2. Methods (The experiment was conducted in accordance with item 2.1.1.10 of the "Disinfection Technical Specifications" (2002 edition))

[0131] (1) Disinfectant solutions with an effective chlorine concentration of 200 mg / L were prepared based on the effective chlorine concentration of the control group, comparative example 1, and examples 4, 6, 7, and 8. The residual disinfectant chemical neutralization method was used to identify the solution. The test was repeated three times.

[0132] (2) Mix the prepared 1.25 times concentration disinfectant solution and the virus suspension with added organic interfering agent according to the method (8:2). The reaction time is 5 min, 10 min and 15 min. After the reaction time is completed, add a neutralizing agent to terminate the reaction, dilute to a safe concentration, and apply to host cells to calculate the titer value. At the same time, use sterile deionized water instead of disinfectant to carry out a positive (virus) control group test. The test is repeated three times.

[0133] (3) The viral titer of each group was determined by the endpoint dilution method, and the average inactivation log value was calculated.

[0134] 3. Regulations for the Evaluation of Virus Inactivation Tests

[0135] If the average inactivation log value of each test is ≥4.00, the laboratory test for disinfection of poliovirus contaminants is deemed qualified.

[0136] 4. Results

[0137] (1) The chlorine-containing disinfectant was prepared in the control group, comparative example 1, and examples 4, 6, 7, and 8. The D / E neutralizing broth can effectively neutralize the residual effect of the disinfectant in the mixture on the poliovirus type 1 (PV-I) vaccine strain. Moreover, the neutralizing agent and the neutralization product have no adverse effects on the poliovirus vaccine strain and cells, indicating that the neutralizing agent is qualified.

[0138] (2) The chlorine-containing disinfectant solution prepared in the control group had an effective chlorine concentration of 50 mg / L. When the solution was applied to the poliovirus vaccine strain for 5 min, 10 min and 15 min, the average kill log value was <4.00, and the virus inactivation effect was not qualified.

[0139] (3) The chlorine-containing disinfectant solution prepared in Comparative Example 1, with an effective chlorine concentration of 200 mg / L, showed an average kill / inactivation log value of <4.00 against the poliovirus vaccine strain after 5 minutes of contact, indicating an unqualified virus inactivation effect. However, after 10 and 15 minutes of contact, the average kill / inactivation log value against the poliovirus vaccine strain was >4.00, indicating a qualified virus inactivation effect. The same solution with an effective chlorine concentration of 100 mg / L showed an average kill / inactivation log value of <4.00 against the poliovirus vaccine strain after 5 and 10 minutes of contact, indicating an unqualified virus inactivation effect. However, after 15 minutes of contact, the average kill / inactivation log value against the poliovirus vaccine strain was >4.00, indicating a qualified virus inactivation effect. Finally, the same solution with an effective chlorine concentration of 50 mg / L showed an average kill / inactivation log value of <4.00 against the poliovirus vaccine strain after 5, 10, and 15 minutes of contact, indicating an unqualified virus inactivation effect.

[0140] (4) The chlorine-containing disinfectant solution prepared in Example 4 had an effective chlorine concentration of 50 mg / L. After acting for 5 min, 10 min and 15 min respectively, the average kill log value of the poliovirus vaccine strain was >4.00, and the virus inactivation effect was qualified.

[0141] (5) The chlorine-containing disinfectant solution prepared in Example 6 with an effective chlorine concentration of 50 mg / L had an average kill and kill log value of <4.00 when acting on the poliovirus vaccine strain for 5 min and 10 min, indicating that the virus inactivation effect was unqualified; when the action time was 15 min, the average kill and kill log value of the poliovirus vaccine strain was >4.00, indicating that the virus inactivation effect was qualified.

[0142] (6) The chlorine-containing disinfectant solutions prepared in Examples 7 and 8 with an effective chlorine concentration of 50 mg / L had an average kill / inactivation log value of <4.00 when acting on the poliovirus vaccine strain for 5 min, indicating that the virus inactivation effect was unqualified; when the action time was 10 min and 15 min, the average kill / inactivation log value of the poliovirus vaccine strain was >4.00, indicating that the virus inactivation effect was qualified.

[0143] (7) Using the chlorine-containing disinfectants prepared in the control group and Examples 4, 6, 7 and 8, when the effective chlorine concentration in the solution was 200 mg / L and 100 mg / L, respectively, after 5 min, 10 min and 15 min, the average kill log value of the poliovirus vaccine strain was >4.00, and the virus inactivation effect was qualified.

[0144] 5. Conclusion

[0145] The chlorine-containing disinfectants prepared in Examples 4, 7, and 8 showed better inactivation effects on the poliovirus vaccine strain than the control group with the same effective chlorine concentration, and were even better than Comparative Example 1. Among them, Example 4 showed the best inactivation effect on the poliovirus vaccine strain (see Table 5).

[0146] Table 5 Virus inactivation effect

[0147]

[0148]

[0149] Based on the above data, the chlorine-containing foam disinfectant effervescent tablets of this invention have excellent killing effects on Staphylococcus aureus, Escherichia coli, and poliovirus type I. Furthermore, their disinfection effect is superior to that of the control group sodium dichloroisocyanurate disinfectant powder and Comparative Example 1. With appropriate addition of a composite surfactant, the foam stability is excellent, improving disinfection visibility and adhesion (adhesion time ≥ 5 min). Simultaneously, the addition of a stabilizer allows the chlorine-containing foam disinfectant effervescent tablets to meet the storage requirements for 2 years, with an effective chlorine reduction rate of < 5% after 72 hours of dissolution in water. The process is simple, transportation is convenient, and it can meet the needs of large-scale farming scenarios such as ranches for low-cost, visually appealing, and easy-to-use disinfection products.

[0150] The above description is merely a preferred embodiment of the present invention, but the scope of protection of the present invention is not limited thereto. Any variations or substitutions that can be easily conceived by those skilled in the art within the technical scope disclosed in the present invention should be included within the scope of protection of the present invention. Therefore, the scope of protection of the present invention should be determined by the scope of the claims.

Claims

1. A chlorine-containing foam disinfectant effervescent tablet, characterized in that, The foam disinfectant effervescent tablets comprise the following components: chlorine-containing disinfectant, compound surfactant, effervescent agent, stabilizer, binder, and filler; the effervescent agent contains an alkaline source and an acid source.

2. The foam disinfectant effervescent tablet according to claim 1, characterized in that, The components and their mass percentages in the foam disinfectant effervescent tablets are as follows: 10-40% chlorine-containing disinfectant, 10-50% compound surfactant, 5-30% effervescent agent, 0-10% stabilizer, 0-5% binder, and the remainder is filler.

3. The foam disinfectant effervescent tablet according to claim 2, characterized in that, The components and their mass percentages in the foam disinfectant effervescent tablets are as follows: 20-40% chlorine-containing disinfectant, 15-40% compound surfactant, 10-30% effervescent agent, 3-10% stabilizer, 0.5-3% binder, and the remainder is filler.

4. The foam disinfectant effervescent tablet according to any one of claims 1-3, characterized in that, The chlorine-containing disinfectant is selected from one or more of sodium dichloroisocyanurate, trichloroisocyanuric acid, and calcium hypochlorite.

5. The foam disinfectant effervescent tablet according to any one of claims 1-3, characterized in that, The composite surfactant is selected from one or more of sodium dodecyl sulfate, sodium fatty acid methyl ester sulfonate, sodium dodecyl sulfonate, sodium dodecylbenzene sulfonate, sodium α-alkenyl sulfonate, sodium cocoyl glutamate, sodium cocoyl hydroxyethyl sulfonate, and sodium lauroyl sarcosinate.

6. The foam disinfectant effervescent tablet according to claim 5, characterized in that, The composite surfactant is a combination of sodium dodecylbenzenesulfonate, sodium fatty acid methyl ester sulfonate, and sodium cocoyl hydroxyethyl sulfonate.

7. The foam disinfectant effervescent tablet according to any one of claims 1-3, characterized in that, The alkaline source in the effervescent agent is selected from one or two of sodium bicarbonate and sodium carbonate; the acid source in the effervescent agent is selected from one or more of malic acid, anhydrous citric acid, sodium bisulfate, boric acid, fumaric acid, adipic acid, cyanuric acid, and aminosulfonic acid.

8. The foam disinfectant effervescent tablet according to any one of claims 1-3, characterized in that, The stabilizer is selected from one or more of sodium tripolyphosphate, sodium pyrophosphate, tetrasodium hydroxyethylidene diphosphonate, aminotrimethylphosphonic acid, 2-hydroxyphosphonoacetic acid, sodium hexametaphosphate, and disodium EDTA.

9. The foam disinfectant effervescent tablet according to any one of claims 1-3, characterized in that, The adhesive is selected from one or more of sodium carboxymethyl cellulose, xanthan gum, carrageenan, hydroxyethyl cellulose, and polyethylene glycol; the filler is selected from one or more of anhydrous glucose, sucrose, lactose, maltodextrin, anhydrous sodium sulfate, and sodium chloride.

10. A method for preparing a chlorine-containing foam disinfectant effervescent tablet as described in any one of claims 1-9, comprising the following steps: Step S2-1: Pass the effervescent agent, stabilizer, binder, and filler through a 20-mesh sieve respectively; Step S2-2: Weigh out the surfactant, effervescent alkali source, part of the binder and filler according to the formula and add them to the mixing equipment. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system A; Step S2-3: Weigh out the chlorine-containing disinfectant, effervescent acid source, stabilizer, and remaining binder according to the formula and add them to the mixing equipment of powder system A. Mix for 10-15 minutes at a speed of 30-100 r / min to obtain powder system B. Step S2-4: Powder system B is granulated using a dry granulation method. The prepared granules are then compressed into tablets using a rotary tablet press, with a tablet weight of 1.0-5.0g, thus obtaining chlorine-containing foam disinfectant effervescent tablets.

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