High-potential potassium hydrogen persulfate substrate modification sheet and preparation method thereof

Abstract

The invention provides a high-potential potassium hydrogen persulfate substrate modified sheet and a preparation method thereof, and relates to the field of substrate modified sheets. Comprising the following components in parts by weight: 10-30 parts of potassium hydrogen persulfate composite salt, 2-3 parts of potassium hydrogen sulfate, 2-5 parts of potassium sulfate, 1-3 parts of sodium chloride, 1-3 parts of polyethylene glycol 60001, 1-3 parts of polyvinylpyrrolidone, 1-3 parts of magnesium sulfate, 3-5 parts of lauryl sodium sulfate, 4-10 parts of sodium metaphosphate and 30-60 parts of sodium sulfate. The invention also provides a method for preparing the high-potential potassium hydrogen persulfate substrate modified sheet. According to the invention, slow dissolution of drugs in a water body is realized through an inclusion technology, active peroxy ions are continuously released, long-acting oxygenolysis of sediment organic matters is ensured, and the continuous demand of an aquaculture environment on sediment improvement is met.

Description

Technical Field

[0001] The present invention relates to the field of preparation of bottom modification sheets, in particular to a high-potential potassium persulfate bottom modification sheet and a preparation method thereof. Background Art

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

[0003] The object of the present invention is to provide a high-potential potassium persulfate bottom modification sheet and a preparation method thereof to solve the above technical problems.

[0004] In order to solve the above technical problems, the present invention adopts the following technical solutions:

[0005] The high-potential potassium persulfate bottom-changing tablet comprises the following components in parts by weight: 10-30 parts of potassium persulfate complex salt, 2-3 parts of potassium hydrogen sulfate, 2-5 parts of potassium sulfate, 1-3 parts of sodium chloride, 1-3 parts of polyethylene glycol 6000, 1-3 parts of polyvinyl pyrrolidone, 1-3 parts of magnesium sulfate, 3-5 parts of sodium lauryl sulfate, 4-10 parts of sodium metaphosphate and 30-60 parts of sodium sulfate.

[0006] One of the preferred components includes the following components in parts by weight: 20 parts of potassium persulfate complex salt, 2 parts of potassium hydrogen sulfate, 3 parts of potassium sulfate, 2 parts of sodium chloride, 1 part of polyethylene glycol 6000, 2 parts of polyvinyl pyrrolidone, 2 parts of magnesium sulfate, 3 parts of sodium lauryl sulfate, 7 parts of sodium metaphosphate and 58 parts of sodium sulfate.

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

[0008] The preparation method of the high-potential potassium persulfate bottom modification sheet comprises the following steps:

[0009] S1, dissolving sodium chloride and polyethylene glycol 6000 in water, stirring magnetically, and spray drying to obtain an inclusion compound;

[0010] S2, placing potassium persulfate, potassium hydrogen sulfate, potassium sulfate, inclusion compound, polyvinyl pyrrolidone, magnesium sulfate, sodium lauryl sulfate, sodium metaphosphate and sodium sulfate into a V-type mixer to obtain a mixture;

[0011] S3. Granulating 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 V-type mixer is used for 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 the present invention are:

[0016] 1. The present invention uses inclusion technology to achieve slow dissolution of drugs in water, continuously release active superoxide ions, ensure long-term oxidative decomposition of organic matter in the bottom mud, and meet the continuous demand for bottom soil improvement in the aquaculture environment.

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

[0018] 3. The optimized formula system increases the redox potential of the aqueous solution by 10% compared with competing products, giving it stronger oxidation ability, which can more efficiently degrade organic matter, kill pathogenic microorganisms, and improve the efficiency of substrate improvement. DETAILED DESCRIPTION

[0019] To facilitate understanding of the present invention, the present invention will be described more fully below. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.

[0020] Unless otherwise defined, all technical and scientific terms used herein have the same meaning as those commonly understood by those skilled in the art of the present invention. The terms used in this specification of the present invention are only for the purpose of describing specific embodiments and are not intended to limit the present invention.

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

[0022] Example 1

[0023] The high-potential potassium persulfate bottom-changing tablets include the following components in parts by weight: 20 parts of potassium persulfate complex salt, 2 parts of potassium hydrogen sulfate, 3 parts of potassium sulfate, 2 parts of sodium chloride, 1 part of polyethylene glycol 6000, 2 parts of polyvinyl pyrrolidone, 2 parts of magnesium sulfate, 3 parts of sodium lauryl sulfate, 7 parts of sodium metaphosphate and 58 parts of sodium sulfate.

[0024] The present invention also provides a method for preparing a 20% high-potential potassium persulfate bottom modification sheet, comprising the following steps:

[0025] S1. Sodium chloride and polyethylene glycol 6000 were dissolved in water, magnetically stirred at 40°C for 1 hour, and spray-dried to obtain an inclusion compound;

[0026] S2, potassium persulfate, potassium hydrogen sulfate, potassium sulfate, inclusion compound, polyvinyl pyrrolidone, magnesium sulfate, sodium lauryl sulfate, sodium metaphosphate and sodium sulfate were placed in a V-type mixer and mixed for 30 minutes to prepare a mixture;

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

[0028] Example 2

[0029] The high-potential potassium persulfate bottom-changing tablets include the following components in parts by weight: 30 parts of potassium persulfate complex salt, 2 parts of potassium hydrogen sulfate, 4 parts of potassium sulfate, 2 parts of sodium chloride, 2 parts of polyethylene glycol 6000, 3 parts of polyvinyl pyrrolidone, 2 parts of magnesium sulfate, 5 parts of sodium lauryl sulfate, 8 parts of sodium metaphosphate and 42 parts of sodium sulfate.

[0030] The present invention also provides a method for preparing a 30% high-potential potassium persulfate bottom modification sheet, comprising the following steps:

[0031] S1. Sodium chloride and polyethylene glycol 6000 were dissolved in water, magnetically stirred at 40°C for 1 hour, and spray-dried to obtain an inclusion compound;

[0032] S2, potassium persulfate, potassium hydrogen sulfate, potassium sulfate, inclusion compound, polyvinyl pyrrolidone, magnesium sulfate, sodium lauryl sulfate, sodium metaphosphate and sodium sulfate were placed in a V-type mixer and mixed for 30 minutes to prepare a mixture;

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

[0034] Example 3

[0035] This example verifies the sterilization effect of the high-potential potassium persulfate bottom modification tablets in Example 1 and Example 2, and 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, centrifugal washing: take 1mL of bacterial suspension and centrifuge (3000rpm, 10 minutes), discard the supernatant, resuspend in PBS buffer, and adjust the concentration to about 10 8 CFU / mL;

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

[0039] S4. Neutralizer 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 of about 10 7 CFU / mL), the action time was set to 5 minutes; ② positive control group: bacterial suspension + PBS buffer (no sterilizer); ③ negative control group: sterile culture medium; ④ neutralizer control group: bacterial suspension + neutralizer (to confirm that the neutralizer has no antibacterial effect);

[0041] S5. Termination of reaction and incubation: After the reaction time is over, neutralizer is added immediately, mixed and allowed to stand for 5 minutes, 100 μL is taken for 10-fold serial dilution, and coated on TSA plates with 3 replicates for each concentration. Staphylococcus aureus is incubated at 37°C for 24 hours, and Aeromonas hydrophila is incubated at 30°C for 24-48 hours;

[0042] S6. Count the colony count (CFU / mL).

[0043] Table 1: Ability of high-potential potassium persulfate tablets to kill hydrophilic monocytes

[0044]

[0045]

[0046] Table 2: Killing ability of high potential potassium persulfate tablets against Staphylococcus aureus

[0047]

[0048] The test data shown in Tables 1 and 2 show that the modified bottom tablets prepared in Examples 1 and 2 can effectively kill Aeromonas hydrophila and Staphylococcus aureus at a minimum dilution of 0.017%, demonstrating their strong killing ability against target pathogens. At the same time, regardless of whether the weight ratio of potassium persulfate complex to the modified bottom tablet is 20% or 30% of the active ingredient, the dilution still maintains a stable bactericidal effect, indicating that the activity of the active ingredient is not significantly affected by concentration differences. This overall shows that the modified bottom tablets prepared by the present invention have the characteristics of strong bactericidal properties, ingredient stability, and economic applicability under experimental conditions.

[0049] Example 4

[0050] This example verifies the stability of the high-potential potassium persulfate bottom modification sheet in Example 1 and Example 2, and the steps are as follows:

[0051] S1. Accelerated test method: Place intact disinfectant samples in a constant temperature and humidity chamber at 45°C and relative humidity >75% for 6 months. Samples are collected for testing before (day 0) and 1 month, 3 months, and 6 months after storage. The measured indicators include the content of the disinfectant's bactericidal active ingredient, solution potential, and pH value. Each sampling must cover samples from three independent production batches. Each batch of samples is tested twice in parallel, and the arithmetic mean is taken as the final result.

[0052] S2. 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. Test process: Accurately weigh approximately 0.4000 g (accurate to ±0.0002 g) and place the sample in a 250 mL iodine volumetric flask. Add appropriate amount of deionized water, 10 mL of sulfuric acid solution and 2.5 g of potassium iodide in sequence. After shaking, seal the bottle mouth and seal with water. Let it react in a dark place for 10 minutes. After opening, rinse the bottle wall with a small amount of deionized water. At room temperature ≤ 25°C, use sodium thiosulfate standard solution to titrate until the solution turns light yellow. After adding 2 mL of starch indicator solution, continue titrating until the blue color fades and the end point color stability is maintained for 30 seconds. Simultaneously carry out a blank control test (except that no sample is added to the blank group, the other reagent types, amounts and operating steps are the same as those of the sample group). Specific test data are shown in Tables 3 and 4.

[0054] Table 3: Stability test data of 20% high potential potassium persulfate bottom modification tablets

[0055]

[0056]

[0057] Table 4: Stability test data of 30% high potential potassium persulfate bottom modification tablets

[0058]

[0059]

[0060] The accelerated stability test data (40°C / RH75%, 6 months) in Tables 3 and 4 show that the 20% and 30% potassium persulfate tablets prepared using inclusion technology exhibit excellent stability. The redox potential values ​​of all samples at concentrations of 1-100 were always maintained above 1100mV, and the potential fluctuation amplitude was less than 1.5% of the initial value. The pH value remained stable. Among them, the relative retention rate of the active ingredient in the 30% high concentration group during the 6-month storage period was as high as 99.2%. The retention rate of the 20% group was 100.3% (initial content 28.62%-29.07%, final value 28.59%-28.86%), and the 20% group also maintained a high retention rate of 99.3%-99.8% (initial content 19.05%-19.84%, final value 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-mentioned embodiments can be combined arbitrarily. In order to make the description concise, not all possible combinations of the technical features in the above-mentioned 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 above-described embodiments merely illustrate several implementations of the present invention, and while their descriptions are relatively specific and detailed, they should not be construed as limiting the scope of the patent. It should be noted that a person skilled in the art would be able to make numerous variations and improvements without departing from the spirit of the present invention, all of which fall within the scope of protection of the present invention. Therefore, the scope of protection of the patent for this invention shall be determined by the appended claims.

Claims

1. High potential potassium persulfate bottom modification sheet, characterized in that, The invention comprises the following components in parts by weight: 10-30 parts of potassium persulfate complex salt, 2-3 parts of potassium hydrogen sulfate, 2-5 parts of potassium sulfate, 1-3 parts of sodium chloride, 1-3 parts of polyethylene glycol 6000, 1-3 parts of polyvinyl pyrrolidone, 1-3 parts of magnesium sulfate, 3-5 parts of sodium lauryl sulfate, 4-10 parts of sodium metaphosphate and 30-60 parts of sodium sulfate.

2. The high-potential potassium persulfate bottom-changing sheet according to claim 1, characterized in that The invention comprises the following components in parts by weight: 20 parts of potassium persulfate complex salt, 2 parts of potassium hydrogen sulfate, 3 parts of potassium sulfate, 2 parts of sodium chloride, 1 part of polyethylene glycol 6000, 2 parts of polyvinyl pyrrolidone, 2 parts of magnesium sulfate, 3 parts of sodium lauryl sulfate, 7 parts of sodium metaphosphate and 58 parts of sodium sulfate.

3. The high potential potassium persulfate bottom modification sheet according to claim 1, characterized in that The invention comprises the following components in parts by weight: 30 parts of potassium persulfate complex salt, 2 parts of potassium hydrogen sulfate, 4 parts of potassium sulfate, 2 parts of sodium chloride, 2 parts of polyethylene glycol 6000, 3 parts of polyvinyl pyrrolidone, 2 parts of magnesium sulfate, 5 parts of sodium lauryl sulfate, 8 parts of sodium metaphosphate and 42 parts of sodium sulfate.

4. The method for preparing the high-potential potassium persulfate bottom-changing sheet according to claim 1, characterized in that: The steps include: S1, dissolving sodium chloride and polyethylene glycol 6000 in water, stirring magnetically, and spray drying to obtain an inclusion compound; S2, potassium persulfate, potassium hydrogen sulfate, potassium sulfate, inclusion compound, polyvinyl pyrrolidone, magnesium sulfate, sodium lauryl sulfate, sodium metaphosphate and sodium sulfate are placed in a V-type mixer and mixed to obtain a mixture; S3. Granulating the mixture.

5. The method for preparing a high-potential potassium persulfate bottom-changing sheet according to claim 4, wherein: Sodium chloride and polyethylene glycol 6000 were dissolved in water and stirred at 40°C for 1 hour.

6. The method for preparing a high-potential potassium persulfate bottom-changing sheet according to claim 4, wherein: The mixing time of the V-type mixer is 30 minutes.

7. The method for preparing a high-potential potassium persulfate bottom-changing sheet according to claim 4, wherein: The dry granulation technology is used to granulate the particles, and the particle size is controlled at 80-120 mesh.

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