High potential potassium peroxymonosulfate modified film and preparation method thereof

Abstract

The application provides a high-potential potassium hydrogen persulfate bottom modification sheet and a preparation method thereof, relates to the field of bottom modification sheets, and comprises the following components in parts by weight: 10-30 parts of potassium hydrogen persulfate composite salt, 2-3 parts of potassium bisulfate, 2-5 parts of potassium sulfate, 1-3 parts of sodium chloride, 1-3 parts of polyethylene glycol 6000, 1-3 parts of polyvinylpyrrolidone, 1-3 parts of magnesium sulfate, 3-5 parts of sodium dodecyl sulfate, 4-10 parts of sodium metaphosphate and 30-60 parts of sodium sulfate. The application also provides a method for preparing the high-potential potassium hydrogen persulfate bottom modification sheet. The application realizes slow dissolution of the drug in water through inclusion technology, continuously releases active peroxide ions, ensures long-acting oxidation and decomposition of the organic matter in the bottom mud, and meets the sustainability requirement of the water product breeding environment for the bottom improvement.

Description

Technical Field

[0001] This invention relates to the field of substrate modification preparation, and more particularly to high-potential potassium peroxymonosulfate substrate modification and its preparation method. Background Technology

[0002] Potassium persulfate is a strong oxidant, and its redox potential is an important indicator of its oxidizing capacity. Potassium persulfate composite salt bottom improvement tablets achieve comprehensive improvement of water quality and bottom environment through multiple mechanisms, including oxidative decomposition of organic matter, sterilization and disinfection, improvement of bottom structure, promotion of beneficial bacteria proliferation, and increased dissolved oxygen. However, current market products generally suffer from technical bottlenecks such as large fluctuations in oxidation potential, slow dissolution rate, and high pH values ​​due to unscientific formulation design and manufacturing process defects. This results in insufficient stability of product oxidation efficiency, and breakthroughs are urgently needed in safety performance indicators and quality controllability. Summary of the Invention

[0003] The purpose of this invention is to provide a high-potential potassium persulfate substrate and its preparation method to solve the above-mentioned technical problems.

[0004] To solve the above-mentioned technical problems, the present invention adopts the following technical solution:

[0005] The high-potential potassium peroxymonosulfate substrate modification sheet comprises the following components in parts by weight: 10-30 parts potassium peroxymonosulfate complex salt, 2-3 parts potassium bisulfate, 2-5 parts potassium sulfate, 1-3 parts sodium chloride, 1-3 parts polyethylene glycol 6000, 1-3 parts polyvinylpyrrolidone, 1-3 parts magnesium sulfate, 3-5 parts sodium dodecyl sulfate, 4-10 parts sodium metaphosphate, and 30-60 parts sodium sulfate.

[0006] One of the preferred components comprises the following components in parts by weight: 20 parts potassium peroxymonosulfate complex salt, 2 parts potassium bisulfate, 3 parts potassium sulfate, 2 parts sodium chloride, 1 part polyethylene glycol 6000, 2 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 3 parts sodium dodecyl sulfate, 7 parts sodium metaphosphate, and 58 parts sodium sulfate.

[0007] Another preferred component includes the following components in parts by weight: 30 parts potassium persulfate complex salt, 2 parts potassium bisulfate, 4 parts potassium sulfate, 2 parts sodium chloride, 2 parts polyethylene glycol 6000, 3 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 5 parts sodium dodecyl sulfate, 8 parts sodium metaphosphate, and 42 parts sodium sulfate.

[0008] The preparation method of the above-mentioned high-potential potassium peroxymonosulfate substrate includes the following steps:

[0009] S1. Dissolve sodium chloride and polyethylene glycol 6000 in water, stir magnetically, and spray dry to obtain inclusion complex;

[0010] S2. Place potassium persulfate complex salt, potassium bisulfate, potassium sulfate, inclusion complex, polyvinylpyrrolidone, magnesium sulfate, sodium dodecyl sulfate, sodium metaphosphate and sodium sulfate into a V-type mixer to obtain a mixture;

[0011] S3. Granulate the mixture.

[0012] Preferably, sodium chloride and polyethylene glycol 6000 are dissolved in water and stirred at 40°C for 1 hour.

[0013] Preferably, the mixing time of the V-type mixer is 30 minutes.

[0014] Preferably, dry granulation technology is used for granulation, and the particle size is controlled at 80-120 mesh.

[0015] The beneficial effects of this invention are:

[0016] 1. This invention utilizes inclusion technology to achieve slow dissolution of the drug in water, continuously releasing active peroxide ions, ensuring long-term oxidative decomposition of organic matter in the bottom sediment, and meeting the continuous needs of aquaculture environments for bottom sediment improvement.

[0017] 2. The inclusion process effectively inhibits the degradation of available oxygen. Under harsh accelerated testing conditions (40℃ / RH75% for 6 months), the main component retention rate is >98.5%, which is significantly better than conventional formulations, ensuring the quality stability of the product during its shelf life.

[0018] 3. The optimized formulation system increases the oxidation-reduction potential of the aqueous solution by 10% compared to competitors, giving it stronger oxidation capabilities, enabling more efficient degradation of organic matter, killing of pathogenic microorganisms, and improving the efficiency of substrate improvement. Detailed Implementation

[0019] To facilitate understanding of the present invention, a more complete description will be provided below. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. Rather, these embodiments are provided to provide a thorough and complete understanding of the disclosure of the present invention.

[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention pertains. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.

[0021] Specific embodiments of the present invention will be described below.

[0022] Example 1

[0023] The high-potential potassium peroxymonosulfate substrate modification sheet comprises the following components in parts by weight: 20 parts potassium peroxymonosulfate complex salt, 2 parts potassium bisulfate, 3 parts potassium sulfate, 2 parts sodium chloride, 1 part polyethylene glycol 6000, 2 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 3 parts sodium dodecyl sulfate, 7 parts sodium metaphosphate, and 58 parts sodium sulfate.

[0024] This invention also provides a method for preparing a 20% high-potential potassium peroxymonosulfate substrate, comprising the following steps:

[0025] S1. Dissolve sodium chloride and polyethylene glycol 6000 in water, stir magnetically at 40°C for 1 hour, and spray dry to obtain the inclusion complex;

[0026] S2. Place potassium persulfate complex salt, potassium bisulfate, potassium sulfate, inclusion complex, polyvinylpyrrolidone, magnesium sulfate, sodium dodecyl sulfate, sodium metaphosphate and sodium sulfate into a V-type mixer and mix for 30 minutes to obtain a mixture;

[0027] S3. Use dry granulation technology to granulate the mixture, and control the particle size to 80 mesh.

[0028] Example 2

[0029] The high-potential potassium peroxymonosulfate substrate modification sheet comprises the following components in parts by weight: 30 parts potassium peroxymonosulfate complex salt, 2 parts potassium bisulfate, 4 parts potassium sulfate, 2 parts sodium chloride, 2 parts polyethylene glycol 6000, 3 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 5 parts sodium dodecyl sulfate, 8 parts sodium metaphosphate, and 42 parts sodium sulfate.

[0030] This invention also provides a method for preparing a 30% high-potential potassium peroxymonosulfate substrate, comprising the following steps:

[0031] S1. Dissolve sodium chloride and polyethylene glycol 6000 in water, stir magnetically at 40°C for 1 hour, and spray dry to obtain the inclusion complex;

[0032] S2. Place potassium persulfate complex salt, potassium bisulfate, potassium sulfate, inclusion complex, polyvinylpyrrolidone, magnesium sulfate, sodium dodecyl sulfate, sodium metaphosphate and sodium sulfate into a V-type mixer and mix for 30 minutes to obtain a mixture;

[0033] S3. Use dry granulation technology to granulate the mixture, and control the particle size to 80 mesh.

[0034] Example 3

[0035] This embodiment verifies the bactericidal effect of the high-potential potassium peroxymonosulfate substrate modification tablets in Examples 1 and 2. The steps are as follows:

[0036] S1. Preparation of bacterial suspension: Staphylococcus aureus and Aeromonas hydrophila were inoculated into TSB medium, respectively. Staphylococcus aureus was cultured at 37°C for 18-24 hours, and Aeromonas hydrophila was cultured at 30°C for 24 hours.

[0037] S2. Centrifugation and washing: Centrifuge 1 mL of bacterial suspension (3000 rpm, 10 minutes), discard the supernatant, resuspend in PBS buffer, and adjust the concentration to approximately 10. 8 CFU / mL;

[0038] S3. Disinfectant dilution: Prepare a gradient concentration of disinfectant, with concentration gradients of 0.05%, 0.025%, 0.02%, and 0.017%, and dilute with PBS;

[0039] S4. Neutralizing agent verification: Verify that sodium thiosulfate can completely neutralize the disinfectant without affecting bacterial growth;

[0040] S5. Sterilization Experiment Design: ① Experimental Group: Bacterial suspension and disinfectant were mixed at a ratio of 1:9 (final bacterial count approximately 10). 7 CFU / mL), with an action time of 5 minutes; ② Positive control group: bacterial suspension + PBS buffer (without sterilizer); ③ Negative control group: sterile culture medium; ④ Neutralizing agent control group: bacterial suspension + neutralizing agent (confirmed that the neutralizing agent has no antibacterial effect);

[0041] S5. Termination of reaction and culture: After the reaction time is over, add the neutralizing agent immediately, mix and let stand for 5 minutes. Take 100 μL and perform a 10-fold serial dilution. Spread the mixture on TSA plates. Perform 3 replicates for each concentration. Incubate Staphylococcus aureus at 37°C for 24 hours and Aeromonas hydrophila at 30°C for 24-48 hours.

[0042] S6. Count the number of colonies (CFU / mL).

[0043] Table 1: Ability of high-potential potassium peroxymonosulfate substrate to kill hydrophilic vapor-producing monocells

[0044]

[0045]

[0046] Table 2: Killing ability of high-potential potassium peroxymonosulfate substrate-modified tablets against Staphylococcus aureus

[0047]

[0048] The experimental data shown in Tables 1 and 2 indicate that the substrate modified tablets prepared in Examples 1 and 2 can effectively kill Aeromonas hydrophila and Staphylococcus aureus at the lowest dilution of 0.017%, demonstrating their extremely strong killing ability against the target pathogens. Furthermore, regardless of whether the weight ratio of potassium persulfate compound salt to substrate modified tablet is 20% or 30% of the active ingredient, the bactericidal effect remains stable after dilution, indicating that the activity of the active ingredient is not significantly affected by concentration differences. In summary, the substrate modified tablets prepared in this invention possess the characteristics of strong bactericidal activity, component stability, and economic applicability under experimental conditions.

[0049] Example 4

[0050] This embodiment verifies the stability of the high-potential potassium peroxymonosulfate substrate modified in Examples 1 and 2. The steps are as follows:

[0051] S1. Accelerated experimental method: The well-packaged disinfectant samples were placed in a constant temperature and humidity chamber at 45℃ and relative humidity >75% for 6 months. Samples were taken and tested before (0 days) and at 1 month, 3 months and 6 months after storage. The test indicators included the content of the effective bactericidal ingredient of the disinfectant, the solution potential value and pH value. Each sampling should cover three independent production batches of samples. Each batch of samples was tested twice in parallel and the arithmetic mean was taken as the final result.

[0052] S2. Preparation of experimental reagents: Potassium iodide, sulfuric acid solution (1:3 volume ratio), sodium thiosulfate standard titration solution [c(Na2S2O3)≈0.1mol / L] and starch indicator solution are required;

[0053] S3. Detection Procedure: Accurately weigh approximately 0.4000g (accurate to ±0.0002g) of the sample and place it in a 250mL iodine flask. Add an appropriate amount of deionized water, 10mL of sulfuric acid solution, and 2.5g of potassium iodide in sequence. Shake well, seal the flask, and allow it to stand in the dark for 10 minutes. After opening, rinse the flask wall with a small amount of deionized water. Under ambient conditions of room temperature ≤25℃, titrate with sodium thiosulfate standard solution until the solution turns pale yellow. Add 2mL of starch indicator solution and continue titrating until the blue color fades and the endpoint color stability is maintained for 30 seconds. Simultaneously conduct a blank control experiment (the blank group is the same as the sample group in terms of reagent types, dosages, and operating procedures, except that no sample is added). For detailed experimental data, please refer to Appendix Tables 3 and 4.

[0054] Table 3: Stability test data of 20% high-potential potassium peroxymonosulfate substrate modified tablets

[0055]

[0056]

[0057] Table 4: Stability test data of 30% high-potential potassium peroxymonosulfate substrate modified tablets

[0058]

[0059]

[0060] Tables 3 and 4 show the accelerated stability test data (40℃ / RH 75%, 6 months), indicating that the 20% and 30% potassium persulfate substrate-modified tablets prepared using inclusion technology exhibited excellent stability. The redox potential of all samples remained above 1100 mV at concentrations ranging from 1 to 100 mV, with potential fluctuations less than 1.5% of the initial value. The pH value remained stable. Notably, the 30% high-concentration group showed a relative retention rate of 99.2% of the active ingredient during 6 months of storage. The initial content was 28.62%-29.07%, and the final content was 28.59%-28.86%. The 20% group also maintained a high retention rate of 99.3%-99.8% (initial content 19.05%-19.84%, final content 19.14%-19.56%). The experiment confirmed that the inclusion technology effectively inhibited the decomposition reaction of potassium persulfate complex salt through intermolecular forces. Under the accelerated conditions of high temperature and high humidity, the effective oxygen degradation rate of all samples was less than 1.5%.

[0061] The technical features of the above embodiments can be combined in any way. For the sake of brevity, not all possible combinations of the technical features in the above embodiments are described. However, as long as there is no contradiction in the combination of these technical features, they should be considered to be within the scope of this specification.

[0062] The embodiments described above are merely illustrative of several implementations of the present invention, and while the descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the invention patent. It should be noted that those skilled in the art can make various modifications and improvements without departing from the concept of the present invention, and these all fall within the protection scope of the present invention. Therefore, the protection scope of this invention patent should be determined by the appended claims.

Claims

1. A high-potential potassium peroxymonosulfate substrate modification film, characterized in that, It consists of the following components in parts by weight: The mixture consists of 10-30 parts potassium peroxymonosulfate compound salt, 2-3 parts potassium peroxymonosulfate, 2-5 parts potassium sulfate, 1-3 parts sodium chloride, 1-3 parts polyethylene glycol 6000, 1-3 parts polyvinylpyrrolidone, 1-3 parts magnesium sulfate, 3-5 parts sodium dodecyl sulfate, 4-10 parts sodium metaphosphate, and 30-60 parts sodium sulfate. The preparation method of high-potential potassium peroxymonosulfate substrate modification film includes the following steps: S1. Sodium chloride and polyethylene glycol 6000 were dissolved in water and then magnetically stirred at 40°C for 1 hour, followed by spray drying to obtain the inclusion complex. S2. Potassium persulfate complex salt, potassium persulfate, potassium sulfate, inclusion complex, polyvinylpyrrolidone, magnesium sulfate, sodium dodecyl sulfate, sodium metaphosphate and sodium sulfate are placed in a V-type mixer and mixed to obtain a mixture; S3. Granulate the mixture.

2. The high-potential potassium peroxymonosulfate substrate modification sheet according to claim 1, characterized in that, It is composed of the following components in parts by weight: 20 parts potassium peroxymonosulfate compound salt, 2 parts potassium bisulfate, 3 parts potassium sulfate, 2 parts sodium chloride, 1 part polyethylene glycol 6000, 2 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 3 parts sodium dodecyl sulfate, 7 parts sodium metaphosphate and 58 parts sodium sulfate.

3. The high-potential potassium peroxymonosulfate substrate modification sheet according to claim 1, characterized in that, It is composed of the following components in parts by weight: 30 parts potassium persulfate compound salt, 2 parts potassium bisulfate, 4 parts potassium sulfate, 2 parts sodium chloride, 2 parts polyethylene glycol 6000, 3 parts polyvinylpyrrolidone, 2 parts magnesium sulfate, 5 parts sodium dodecyl sulfate, 8 parts sodium metaphosphate and 42 parts sodium sulfate.

4. The high-potential potassium peroxymonosulfate substrate modification sheet according to claim 1, characterized in that, The V-type mixer has a mixing time of 30 minutes.

5. The high-potential potassium peroxymonosulfate substrate modification sheet according to claim 1, characterized in that, Dry granulation technology is used for granulation, and the particle size is controlled at 80-120 mesh.

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