Preparation method of a juglone solid pesticide and insecticidal activity thereof

Abstract

The present application belongs to the technical field of plant source pesticide, and relates to a preparation method of juglone solid pesticide and insecticidal activity of the same, in particular to a preparation method of juglone effervescent tablets and insecticidal activity of the same. The prescription composition of the juglone effervescent tablets is as follows in terms of mass percentage: 5-20% of juglone, 30-75% of effervescent agent, 5-25% of dispersing agent, 5-35% of inert carrier and 0-10% of lubricant. Compared with traditional chemical pesticides, the effervescent tablet of the present application belongs to 'green pesticide', has good chemical and physical stability, avoids decomposition of the original medicine, has no organic solvent and emulsifier compared with traditional pesticide dosage form, has good safety, small environmental pollution, is convenient to store, transport and use, has short disintegration and dispersion time, and has good insecticidal activity.

Description

Technical Field

[0001] This invention belongs to the field of plant-derived pesticide technology, and relates to a method for preparing a solid juglone pesticide and its insecticidal activity, specifically to a method for preparing juglone effervescent tablets and its insecticidal activity. Background Technology

[0002] Juglans regia contains a biologically active chemical substance called juglone, chemically known as 5-hydroxy-1,4-naphthoquinone, with the molecular formula: C 10 H6O3, with a molecular weight of 174.16, is an insecticidal chemical. my country is a major agricultural country, using large quantities of chemical pesticides annually. Long-term pesticide use has caused environmental pollution and harm to human health. With social development, people are paying increasing attention to environmental safety, creating an urgent need to develop environmentally friendly green pesticide formulations. With the continuous development of ultra-efficient pesticides, research on new pesticide formulations has also progressed rapidly. Numerous studies have shown that highly efficient, safe, economical, and easy-to-use new pesticide formulations are emerging. Formulations that meet the criteria for green pesticide formulations include: effervescent tablets, microemulsions, and water-in-oil emulsions.

[0003]

[0004] Pesticides, as a major agricultural input, play a vital role in controlling crop diseases, pests, and weeds and ensuring agricultural harvests. Although integrated pest management and the promotion and application of genetically modified crops have achieved great success, pesticides will remain irreplaceable for a considerable period. my country is a major agricultural country, using approximately 3.5 million tons of pesticides annually, more than half of which are traditional chemical pesticides. These pesticides typically require the addition of organic solvents such as benzene, toluene, xylene, methanol, and dimethylformamide. These solvents are highly volatile and toxic, posing extremely high risks during transportation, storage, and use. Most importantly, they pollute soil and aquatic environments, causing serious harm to mammals, aquatic organisms, and non-target organisms. For example, using 1 ton of 4.5% high-efficiency cypermethrin emulsifiable concentrate is equivalent to injecting 850 kilograms of xylene into the environment, demonstrating the severity of its environmental pollution. Therefore, these traditional pesticide formulations can no longer meet the increasingly stringent safety regulations, necessitating the vigorous development of environmentally friendly green pesticide formulations to adapt to current international environmental protection requirements.

[0005] Compared to conventional chemical pesticides, plant-derived pesticides have the advantages of being environmentally friendly, having diverse biological activities, being less likely to induce pesticide resistance in pests, and being relatively safe for non-target organisms. Their environmental friendliness is mainly due to the fact that plant-derived pesticides originate from nature, are more easily decomposed after application, and cause little or no pollution to the environment.

[0006] Effervescent tablets are a novel pesticide formulation, a special type of tablet with pesticide as the main ingredient. They are tablets that automatically disintegrate in water to form a suspension for spraying. In addition to the active ingredient, effervescent tablets contain fillers, binders, wetting agents, dispersants, disintegrants, and lubricants. The difference between effervescent tablets and ordinary tablets is the addition of a disintegrant in the formulation. Effervescent tablets generally use an acid-base system as their disintegrant, i.e., an acid source and a carbon dioxide source.

[0007] The effectiveness of pesticide effervescent tablets depends not only on the main components of the pesticide, but also on the excipients, fillers, wetting agents, dispersants, disintegrants, binders, etc. in the pesticide tablets.

[0008] There are no existing reports on the preparation of juglone into effervescent tablets for insecticidal purposes. Summary of the Invention

[0009] To overcome the shortcomings of existing technologies, the technical problem solved by this invention is to provide a method for preparing juglone effervescent tablets and their insecticidal activity. The prepared juglone effervescent tablets are in tablet form, making them extremely convenient to use; simply dissolve the tablets in water. Compared with traditional chemical pesticides, they have advantages such as being environmentally friendly, producing no dust, exhibiting diverse biological activities, being less likely to induce resistance, and being relatively safe for non-target organisms.

[0010] This invention is implemented according to the following technical solution:

[0011] A solid pesticide containing juglone, wherein the solid pesticide containing juglone is a juglone effervescent tablet.

[0012] Furthermore, the formulation composition of the juglone effervescent tablets, by mass percentage, is as follows: juglone 5-20%, effervescent agent 30-75%, dispersant 5-25%, inert carrier 5-35%, and lubricant 0-10%.

[0013] Furthermore, the formulation composition of the juglone effervescent tablets, by mass percentage, is as follows: juglone accounts for 6-15%, effervescent agent accounts for 40-65%, dispersant accounts for 6-20%, inert carrier accounts for 10-30%, and lubricant accounts for 0-5%.

[0014] Furthermore, the formulation of the juglone effervescent tablets, by mass percentage, is as follows: juglone accounts for 8-12%, effervescent agent accounts for 55-65%, dispersant accounts for 6-10%, inert carrier accounts for 15-25%, and lubricant accounts for 0-2%.

[0015] Furthermore, the mass ratio of juglone to the inert carrier is 1:0.5-2, preferably 1:1.5-2.

[0016] Furthermore, the effervescent agent is composed of an acid source and an alkaline source.

[0017] The molar ratio of the acid source to the base source is 3:5 to 3:7.

[0018] The mass ratio of the dispersant to the alkali source is 1:2-6.

[0019] Furthermore, the acid source includes one or more combinations of anhydrous citric acid, adipic acid, tartaric acid, succinic acid, malic acid, and glutaric acid; the alkali source includes one or more combinations of sodium carbonate, sodium bicarbonate, sodium percarbonate, potassium carbonate, and calcium carbonate.

[0020] Furthermore, the effervescent agent is preferably a combination of one of anhydrous citric acid, adipic acid, tartaric acid, and malic acid with sodium carbonate, or a combination of one of anhydrous citric acid, adipic acid, tartaric acid, and malic acid with sodium bicarbonate, or a combination of anhydrous citric acid with sodium bicarbonate and sodium carbonate.

[0021] Furthermore, the inert carrier is one or a combination of several of the following: silica (white carbon black), diatomaceous earth, charcoal, organobentonite, kaolin, and light calcium carbonate.

[0022] Depending on the adsorption properties of the inert carrier, the particle size of the inert carrier used is 800±80 mesh to 2000±200 mesh.

[0023] Specifically, when silica is used as an inert carrier, its particle size is 2000±200 mesh;

[0024] When diatomaceous earth is used as an inert carrier, its particle size is 800±80 mesh;

[0025] When kaolin is used as an inert carrier, its particle size is 800±80 mesh;

[0026] When light calcium carbonate is used as an inert carrier, its particle size is 1000±100 mesh.

[0027] Further, the dispersant is one or more of the following: polyethylene glycol 2000, polyethylene glycol 4000, polyethylene glycol 6000, polyethylene glycol 8000, polyvinylpyrrolidone K30, polyvinylpyrrolidone K90, and polyvinyl alcohol 0588.

[0028] Furthermore, the lubricant is one or more of the following: talc, polyethylene glycol 1000, and sodium dodecyl sulfate.

[0029] Except for the inert carrier, the particle size of the other components is not particularly important and can be within the normal range. The particle size has no significant effect on the properties of juglone effervescent tablets.

[0030] Furthermore, the present invention provides a method for preparing the juglone effervescent tablets, the specific steps of which are as follows:

[0031] 1) Dissolve the prescribed amount of juglone in an organic solvent, add it to an inert support, and load the juglone onto the inert support with stirring. Recover the organic solvent to obtain the precipitate;

[0032] 2) Mix the alkali source with a portion of the dispersant evenly to prepare alkali source particles;

[0033] 3) The precipitate from 1) and the alkali source particles from 2) are mixed by a rolling process to obtain granules;

[0034] 4) Mix the granules obtained in 3) with the acid source, the remaining dispersant and lubricant evenly, and compress into tablets to obtain the final product.

[0035] In step 1), the organic solvent is benzene, chloroform, or dichloromethane, preferably dichloromethane.

[0036] The mass ratio of juglone to the inert carrier is 1:0.5-2.

[0037] This invention provides the application of the aforementioned juglone effervescent tablets in the preparation of pesticides.

[0038] This invention provides the application of the aforementioned juglone effervescent tablets in the preparation of insecticides.

[0039] Furthermore, the insecticide is a pesticide used to kill diamondback moth larvae, cabbage caterpillars, or tea geometrid moth larvae.

[0040] Method of using the juglone effervescent tablets described in this invention:

[0041] Dissolve one effervescent tablet in water to prepare an aqueous solution of the desired concentration. Then spray the solution on plants or crops containing cabbage caterpillars, tea geometrid moth larvae, or false-eyed green leafhoppers.

[0042] Preparation methods include concentrated and diluted methods. One method involves directly preparing an aqueous solution of the desired concentration from one effervescent tablet, while another involves first preparing an aqueous solution of a certain concentration from one effervescent tablet and then diluting it to the desired concentration. It must be prepared immediately before use.

[0043] The beneficial effects of this invention are:

[0044] This invention provides an effervescent tablet with juglone as the main active ingredient. Compared with traditional chemical pesticides, the effervescent tablet of this invention is a "green pesticide" with good chemical and physical stability, avoiding the decomposition of the active ingredient; compared with traditional pesticide formulations, it does not contain organic solvents and emulsifiers, has good safety, and causes less environmental pollution; it is easy to store, transport and use; it has a short disintegration and dispersion time and good insecticidal activity. Detailed Implementation

[0045] The present invention prepares juglone solid pesticide according to the following method.

[0046] Process 1: A method for preparing juglone solid pesticide, the specific steps of which are as follows:

[0047] (1) Dissolve 100g of juglone in an organic solvent, add 200g of silica, stir for 2 hours, recover dichloromethane under reduced pressure, and pulverize the resulting precipitate to 60-80 mesh for later use.

[0048] (2) Mix a certain amount of dispersant with an alkali source evenly, and prepare particles by heating and melting and then cooling, or dissolve the dispersant and alkali source in an organic solvent and prepare particles by non-aqueous solvent. After drying, pulverize to 40-60 mesh particles for later use. The alkali source is sodium bicarbonate.

[0049] (3) After mixing the particles obtained from (1) and (2) evenly, the mixed particles are prepared by rolling.

[0050] (4) Mix the particles obtained in (3), acid source (controlling water content), dispersant and lubricant evenly, wherein the acid source is anhydrous citric acid.

[0051] (5) In an environment with humidity <30% and temperature <25℃, the mixture obtained in (4) is pressed by adjusting the pressing parameters of the rotary tablet press to obtain 200 juglone effervescent tablets.

[0052] Prescription screening:

[0053] 1. Selection of silica particle size in step (1)

[0054] Solid juglone pesticides were prepared by using 500-mesh, 1000-mesh, and 2000-mesh silica as carriers, respectively, according to process 1.

[0055] The suspension rates of juglone supported on silica with three different particle sizes were investigated. The results showed that within one hour, the suspension rates of juglone supported on 500-mesh, 1000-mesh, and 2000-mesh silica were 22%, 67%, and 98%, respectively. Relatively speaking, the finer the particle size of the silica, the stronger its ability to support juglone. Therefore, 2000-mesh silica was preferred as an inert support, and its loading capacity did not change significantly within a particle size range of 2000 ± 200 mesh.

[0056] 2. Selection of organic solvent in step (1)

[0057] Juglone is poorly soluble in water but readily soluble in organic solvents such as benzene and chloroform. Dissolving juglone in an organic solvent before adsorption onto an inert support allows for better adsorption onto the inert support surface, increasing dispersion and solubility. Since benzene and chloroform are highly toxic and detrimental to production, dichloromethane, with slightly lower solubility but also lower toxicity, was chosen as the solvent for juglone. Dichloromethane not only has low toxicity but also meets the dissolution requirements and is more conducive to vacuum recovery.

[0058] 3. Selection of dispersant

[0059] Preliminary test results show that PEG-based dispersants can achieve good dispersion effects. The following is a further screening of the formulation using PEG4000 as a dispersant.

[0060] 4. Orthogonal experimental design

[0061] Based on the aforementioned process conditions, the drug / inert carrier mass ratio (A), acid / alkali molar ratio (B), and dispersant amount were selected as influencing factors (C), and three levels were set for each. Juglone effervescent tablets were prepared according to the method of Process 1. A three-factor, three-level orthogonal design was designed to screen the formulation, using the comprehensive score of disintegration time and suspension rate as the index.

[0062] Overall score = (Disintegration time score * 50%) + (Suspension rate score * 50%)

[0063] Disintegration Time Score = Shortest Disintegration Time in this Group / Disintegration Time in this Session * 100

[0064] Suspension rate score = (Suspension rate of this group / Highest suspension rate of this group) * 100

[0065] (1) The factors and their levels are shown in Table 1:

[0066] Table 1. Factors and Levels

[0067] Factors and Levels Drug / carrier mass ratio (A) Acid source / base source molar ratio (B) Amount of dispersant (C) Low 1∶2 3∶7 10％ middle 1∶1 3∶5 15％ high 2∶1 3∶3 20％

[0068] Table 2 Orthogonal array and results

[0069]

[0070] The results of the orthogonal experiment show that the influence of the factors is in the following order: B>A>C, that is: acid source / base source molar ratio>drug / carrier ratio>amount of dispersant;

[0071] Disintegration time and suspension rate were used as evaluation indicators, with shorter disintegration time and higher suspension rate being preferred. Specifically, a disintegration time of less than 60 seconds and a suspension rate of greater than 90% both met the preparation requirements of the effervescent tablets of this invention. The results showed that when silica was used as an inert carrier, PEG4000 as a dispersant, and a combination of anhydrous citric acid and sodium bicarbonate as an effervescent agent, the drug / carrier mass ratio was 1:0.5-2, the acid source / alkali source molar ratio was 3:5-3:7, and the amount of dispersant was 10%-20%, the disintegration time of the prepared effervescent tablets was within 60 seconds, and the suspension rate was greater than 90%.

[0072] Furthermore, the orthogonal experimental results show that the optimal combination is formulation A1B2C1, which is: drug / carrier ratio of 1:2, acid / base molar ratio of 3:5, and dispersant content of 10%.

[0073] Example 1

[0074] Taking the production of 200 pieces as an example:

[0075] prescription:

[0076]

[0077] Process:

[0078] Juglone was dissolved in 500 mL of dichloromethane, and 200 g of silica was added under stirring. The mixture was stirred in a sealed container for 2 hours, and the dichloromethane was recovered by vacuum distillation at 35 °C. The resulting precipitate was pulverized and passed through an 80-mesh sieve for later use.

[0079] Heat 80g of PEG4000 in a water bath at 60℃ until it melts. Add sodium bicarbonate powder while stirring, stir until homogeneous, remove, cool to room temperature, and then pulverize through a 40-mesh sieve for later use.

[0080] After mixing the granules obtained in the above two steps, they are pressed into thin sheets of 1-1.2 mm thickness using a roller press, then crushed and passed through a 24-mesh sieve for later use.

[0081] 10g of PEG4000 was dissolved in 100mL of anhydrous ethanol and sprayed onto the surface of anhydrous citric acid granules with stirring. After the anhydrous ethanol evaporated naturally, the granules and the remaining PEG4000 were placed in a three-dimensional mixer and mixed for 10min. The mixture was then removed and pressed into juglone effervescent tablets with a thickness of 3.8mm and a tablet output speed of 1 tablet / second using a rotary tablet press under conditions of 28% humidity and 23℃. The tablets were then pressed with a Φ10mm punch to produce 5g tablets of juglone effervescent tablets.

[0082] The effervescent tablets disintegrated in 40 seconds at 25°C, with a suspension rate of 96.2%.

[0083] The resulting effervescent tablets were stored in independent, airtight packaging using aluminum-plastic composite materials under the same temperature and humidity conditions.

[0084] Example 2

[0085] Taking the production of 200 pieces as an example:

[0086] prescription:

[0087]

[0088] Process:

[0089] Juglone was dissolved in 500 mL of dichloromethane, and 200 g of diatomaceous earth powder was added under stirring. The mixture was stirred in a sealed container for 2 hours, and the dichloromethane was recovered by vacuum distillation at 35 °C. The resulting precipitate was pulverized and passed through an 80-mesh sieve for later use.

[0090] Dissolve 75g of polyvinylpyrrolidone K30 in 500ml of 95% ethanol. Add sodium carbonate powder while stirring and stir until evenly mixed. Remove the powder and place it on a sieve to air dry naturally. Dry it in a 40℃ oven until the moisture content is less than 3%. Remove the powder and grind it through a 40-mesh sieve for later use.

[0091] After mixing the granules obtained in the above two steps, they are pressed into thin sheets of 1-1.2 mm using a roller press, then crushed and passed through a 24-mesh sieve for later use.

[0092] Dissolve 5g of polyvinylpyrrolidone K30 in 100ml of anhydrous ethanol, and spray it onto the surface of tartaric acid particles while stirring. After the ethanol evaporates naturally, place the particles and PEG1000 in a three-dimensional mixer and mix for 12 minutes. Under conditions of 30% humidity and 23℃, adjust the rotary tablet press to a thickness of 4.0mm and adjust the tablet output speed to 1 tablet / second. Press juglone effervescent tablets weighing 5g with a Φ10mm punch to obtain the product.

[0093] The effervescent tablets tested disintegrated in 45 seconds at 25°C, with a suspension rate of 97.6%.

[0094] The resulting effervescent tablets were stored in independent, airtight packaging using aluminum-plastic composite materials under the same temperature and humidity conditions.

[0095] Example 3

[0096] Taking the production of 200 pieces as an example:

[0097] prescription:

[0098]

[0099] Process:

[0100] Juglone was dissolved in 500 mL of dichloromethane, and 200 g of light calcium carbonate was added under stirring. The mixture was stirred in a sealed container for 2 hours, and the dichloromethane was recovered by vacuum distillation at 35 °C. The resulting precipitate was pulverized and passed through an 80-mesh sieve for later use.

[0101] Dissolve 55g of polyvinyl alcohol 0588 in 500ml of 95% ethanol. Add sodium bicarbonate powder while stirring, stir until evenly mixed, remove and place on a sieve to air dry naturally. Dry in a 40℃ oven until the moisture content is less than 3%. Remove and grind through a 40-mesh sieve for later use.

[0102] After mixing the granules obtained in the above two steps, they are pressed into thin sheets of 1-1.2 mm using a roller press, then crushed and passed through a 24-mesh sieve for later use.

[0103] 5g of polyvinyl alcohol 0588 was dissolved in 50mL of anhydrous ethanol and sprayed onto the surface of malic acid granules (60 mesh) under stirring. After the ethanol evaporated naturally, the granules and talc were placed in a three-dimensional mixer and mixed for 10min. The mixture was then removed and pressed into juglone effervescent tablets with a thickness of 4.1mm and a tablet output speed of 1 tablet / second using a rotary tablet press at 30% humidity and 23℃. The tablets weighing 5g were then pressed using a Φ10mm punch.

[0104] The effervescent tablets tested disintegrated in 32 seconds at 25°C, with a suspension rate of 98.1%. The resulting effervescent tablets were stored in individually sealed aluminum-plastic packaging under the same temperature and humidity conditions.

[0105] Example 4

[0106] Taking the production of 200 pieces as an example:

[0107] prescription:

[0108]

[0109]

[0110] Process:

[0111] Juglone was dissolved in 500 mL of dichloromethane, and 200 g of 2000 mesh silica was added under stirring. The mixture was stirred in a sealed container for 2 hours, and the dichloromethane was recovered by vacuum distillation at 35 °C. The resulting precipitate was pulverized and passed through an 80 mesh sieve for later use.

[0112] Take 70g of PEG2000, heat it to 60℃ to dissolve it, add sodium bicarbonate and sodium carbonate powder while stirring, stir evenly, take it out, cool it to room temperature, and grind it through a 40-mesh sieve for later use.

[0113] After mixing the granules obtained in the above two steps, they are pressed into thin sheets of 1-1.2 mm using a roller press, then crushed and passed through a 24-mesh sieve for later use.

[0114] 10g of PEG2000 was prepared into a 10% anhydrous ethanol solution and sprayed onto the surface of anhydrous citric acid granules (80 mesh) under stirring. After the ethanol evaporated, the granules and talc were mixed in a three-dimensional mixer for 1 minute. The mixture was then removed and pressed into juglone effervescent tablets with a thickness of 3.7mm and a tablet output speed of 1 tablet / second using a rotary tablet press at 30% humidity and 23℃. The tablets weighing 5g were then pressed using a Φ10mm punch.

[0115] The effervescent tablets tested disintegrated in 38 seconds at 25°C, with a suspension rate of 97.4%.

[0116] The resulting effervescent tablets were stored in independent, airtight packaging using aluminum-plastic composite materials under the same temperature and humidity conditions.

[0117] Example 5

[0118] Taking the production of 200 pieces as an example:

[0119] prescription:

[0120]

[0121]

[0122] Process:

[0123] Juglone was dissolved in 500 mL of dichloromethane, and 200 g of 200 mesh kaolin was added under stirring. The mixture was stirred in a sealed container for 2 hours, and the dichloromethane was recovered by vacuum distillation at 35 °C. The resulting precipitate was pulverized and passed through an 80 mesh sieve for later use.

[0124] Take the prescribed amount of PEG2000, heat it to 60℃ to dissolve it, add sodium bicarbonate powder while stirring, stir evenly, remove it, cool it to room temperature, and grind it through a 40-mesh sieve for later use.

[0125] After mixing the granules obtained in the above two steps, they are pressed into thin sheets of 1-1.2 mm using a roller press, then crushed and passed through a 24-mesh sieve for later use.

[0126] Prepare a 10% anhydrous ethanol solution using the prescribed amount of PVPk30. Spray the solution onto the surface of adipic acid (60 mesh) particles while stirring. After the ethanol has evaporated, mix the particles with the adipic acid particles in a three-dimensional mixer for 10 minutes. Under conditions of 30% humidity and 23°C, adjust the rotary tablet press to a thickness of 3.8 mm and a tablet output speed of 1 tablet / second. Press 5 g of juglone effervescent tablets using a Φ10 mm punch to obtain the final product.

[0127] The effervescent tablets tested disintegrated in 42 seconds at 25°C, with a suspension rate of 98.8%. The resulting effervescent tablets were stored in individually sealed aluminum-plastic packaging under the same temperature and humidity conditions.

[0128] Examples 2-5 show that, referring to Example 1, by changing the components and contents of each effervescent tablet, effervescent tablets with a disintegration time of less than 60s and a suspension rate of more than 95% can be obtained, which meets the preparation requirements of effervescent tablets.

[0129] Example 6: Insecticidal activity of juglone effervescent tablets

[0130] 1. Methods: The stomach poison toxicity of juglone microemulsion to cabbage caterpillar, tea geometrid moth larva, and false-eyed green leafhopper was tested using the poison bait method.

[0131] 2. Experimental Materials and Equipment

[0132] (1) Experimental materials:

[0133] Test reagent: Juglone effervescent tablets prepared according to the formulation and process of Examples 1-5.

[0134] Test insects: diamondback moth larvae, cabbage caterpillars, and tea geometrid moth larvae raised indoors without exposure to pesticides.

[0135] (2) Experimental equipment: petri dishes, filter paper, distilled water, cabbage leaves, tea leaves, etc.

[0136] 3. Experimental Procedure

[0137] (1) At room temperature, one effervescent tablet of each of Examples 1-5 was placed in distilled water. After effervescence, the juglone effervescent tablet solutions of each example were diluted to 200 μg / mL, 100 μg / mL, 50 μg / mL, 25 μg / mL and 12.5 μg / mL respectively. The control was distilled water.

[0138] (2) Place filter paper at the bottom of the petri dish, add a small amount of distilled water to wet it evenly, and mark it.

[0139] (3) Inoculate 20 test insects into each culture dish, and repeat each treatment or control 3 times.

[0140] (4) After soaking the leaf disc in the drug solution or distilled water for 5-10 seconds, take it out, air dry it, and place it in a petri dish with the corresponding concentration marking.

[0141] (5) After 24 hours, observe the experimental results, calculate the mortality rate and corrected mortality rate (both are the average of 3 replicates), and calculate the toxicity regression equation to determine the LC. 50 value.

[0142] 4. Results and Calculations

[0143] Check the insect survival and mortality status and LC after 24 hours. 50 The values ​​are shown in Table 1-5.

[0144] Table 1. Insect survival and mortality rates and LC2 24 hours after pesticide application in Example 1 50

[0145]

[0146] Table 2. Insect survival and mortality rates and LC50 24 hours after pesticide application in Example 2.

[0147]

[0148] Table 3. Insect survival and mortality rates and LC50 24 hours after pesticide application in Example 3.

[0149]

[0150] Table 4. Insect survival and mortality rates and LC50 24 hours after pesticide application in Example 4.

[0151]

[0152] Table 5. Insect survival and mortality rates and LC50 24 hours after pesticide application in Example 5.

[0153]

[0154] The results above indicate that the juglone effervescent tablets of Examples 1-5 all exhibit significant insecticidal activity against diamondback moth larvae, cabbage caterpillars, and tea geometrid moth larvae.

[0155] When the concentration of the pesticide solution was 12.5-200 μg / mL, Examples 1-5 all showed good killing effects on diamondback moth larvae, cabbage caterpillars, and tea geometrid moth larvae. At a concentration of 100-200 μg / mL, a kill rate of over 85% was achieved. When the concentration was increased to 200 μg / mL, the kill rate of each example against various pests reached over 90%, especially Examples 1, 2, 3, and 5, which achieved a kill rate of 95%, almost completely eliminating the pests.

[0156] With LC 50 As an indicator, the formulation of Example 3 showed better performance compared to other formulations.

Claims

1. A juglone solid pesticide, characterized in that: The juglone solid pesticide is a juglone effervescent tablet containing juglone, an effervescent agent, a dispersant, an inert carrier, and a lubricant. By mass percentage, juglone accounts for 5-20%, the effervescent agent for 30-75%, the dispersant for 5-25%, the inert carrier for 5-35%, and the lubricant for 0-10%.

2. The juglone solid pesticide according to claim 1, characterized in that: By mass percentage, juglone accounts for 6-15%, effervescent agent accounts for 40-65%, dispersant accounts for 6-20%, inert carrier accounts for 10-30%, and lubricant accounts for 0-5%.

3. The juglone solid pesticide according to claim 1, characterized in that: By mass percentage, juglone accounts for 8–12%, effervescent agent accounts for 55–65%, dispersant accounts for 6–10%, inert carrier accounts for 15–25%, and lubricant accounts for 0–2%.

4. A juglone solid pesticide according to any one of claims 1-3, characterized in that: The effervescent agent comprises an acid source and an alkali source. The acid source includes one or more combinations of citric acid, adipic acid, tartaric acid, succinic acid, malic acid, and glutaric acid. The alkali source includes one or more combinations of sodium carbonate, sodium bicarbonate, sodium percarbonate, potassium carbonate, and calcium carbonate. The dispersant includes one or more combinations of polyethylene glycol 2000, polyethylene glycol 4000, polyethylene glycol 6000, polyethylene glycol 8000, polyvinylpyrrolidone K30, polyvinylpyrrolidone K90, and polyvinyl alcohol 0588. The lubricant is one or more combinations of talc, polyethylene glycol 1000, and sodium dodecyl sulfate.

5. A juglone solid pesticide according to any one of claims 1-3, characterized in that: The effervescent agent is a combination of one of anhydrous citric acid, adipic acid, tartaric acid, and malic acid with sodium carbonate, or a combination of one of anhydrous citric acid, adipic acid, tartaric acid, and malic acid with sodium bicarbonate, or a combination of anhydrous citric acid with sodium bicarbonate and sodium carbonate.

6. A juglone solid pesticide according to any one of claims 1-3, characterized in that: The mass ratio of juglone to the inert carrier is 1:0.5-2, preferably 1:1.5-2.

7. The juglone solid pesticide according to claim 4, characterized in that: The molar ratio of the acid source to the base source is 3:5 to 3:

7.

8. The method for preparing the juglone solid pesticide according to claim 1, characterized in that, Includes the following steps: 1) Dissolve the prescribed amount of juglone in an organic solvent, add it to an inert support, load the juglone onto the inert support with stirring, recover the organic solvent, and obtain the precipitate; 2) Mix the alkali source with a portion of the dispersant evenly to prepare alkali source particles; 3) The precipitate from 1) and the alkali source particles from 2) are mixed by a rolling process to obtain granules; 4) Mix the granules obtained in 3) with the acid source, the remaining dispersant and lubricant evenly, and compress into tablets to obtain the final product.

9. The use of the juglone solid pesticide according to any one of claims 1-7 in the preparation of pesticides.

10. The use of the juglone solid pesticide according to any one of claims 1-7 in the preparation of an insecticide, wherein the insecticide is preferably an insecticide for killing diamondback moth larvae, cabbage caterpillars, or tea geometrid moth larvae.

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