A ring-shaped pesticide slow-release agent, its preparation method and application

By using ring-shaped pesticide sustained release agents made of chitosan and other sustained release materials, the problem of traditional sprayed pesticides being difficult to prevent and control fall armyworms during the corn ear-bearing period is solved, and the slow release in humid environments is achieved, which significantly improves the prevention and control effect and reduces pesticide waste.

CN112021318BActive Publication Date: 2025-05-27HUICHUANG (JINAN) TECH SERVICE CO LTD
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Patent Information

Application Number
CN202010852390.0
Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Filing Date
2020-08-21
Publication Date
2025-05-27
Estimated Expiration
2040-08-21

AI Technical Summary

Technical Problem

The prior art spraying chemical pesticides during the corn ear-bearing period is difficult to effectively prevent and control the fall armyworm. Traditional sprays are easily washed away by rainwater, causing pesticide waste and also have a negative impact on beneficial organisms.

Method used

The ring-shaped pesticide sustained release agent made of chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate, calcium chloride and other sustained release materials, forms a three-dimensional network space structure to surround the pesticide active agent and make an elastic ring, which can slowly release insecticidal active ingredients in humid environments.

Benefits of technology

It significantly improves the prevention and treatment effect of fall armyworm and corn ear rot, reduces the amount of pesticides, extends the prevention and control time, and reduces the impact on the environment and beneficial organisms.

✦ Generated by Eureka AI based on patent content.

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Abstract

The present invention discloses an annular pesticide slow-release agent, which comprises an elastic ring. The elastic ring comprises the following raw material components by weight percentage: 0.1-2.0% of a pesticide active agent, 1%-10.0% of an organic solvent, 2.15%-6.7% of a slow-release material, 5%-20.0% of a plant essential oil, 0.1%-0.5% of an emulsifier, 0.01%-0.05% of an organic acid, and the balance is water; the slow-release material comprises chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride. The annular pesticide slow-release agent of the present invention can slowly release the pesticide active ingredients under humid environments or rain leaching conditions, has good control effects on diseases such as maize ear rot and pests such as Spodoptera frugiperda, can significantly improve the insecticidal control effect, reduce the dosage of pesticides, and extend the pesticide prevention and control time, thereby safeguarding the safety of grain production.
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Description

Technical Field

[0001] The present invention relates to the technical field of pesticides, and specifically relates to an annular pesticide slow-release agent, a preparation method thereof, and an application thereof. Background Art

[0002] The fall armyworm, also known as the autumn armyworm, belongs to the order Lepidoptera, family Noctuidae, genus Spodoptera, and is a polyphagous pest native to the tropical and subtropical regions of the Americas. The larvae can feed on 353 plant species in 76 families such as corn, sugarcane, sorghum, and millet, and spread and cause damage in many countries, causing huge losses in Brazil and Africa. Since its invasion in 2019, the fall armyworm has been found in 25 provinces, autonomous regions, and municipalities directly under the Central Government in China, with an area of more than 15 million mu where the insects are seen, and the actual damaged area is 2.68 million mu. Studies have found that the feeding and damage habit of the fall armyworm aggregating on corn ears not only causes direct yield losses, but also the granular excrement is mixed among the grains, which will aggravate the occurrence of plant diseases, resulting in a significant reduction in the yield and quality of corn and causing greater economic losses.

[0003] At present, the prevention and control of the fall armyworm mainly rely on chemical agents. However, during the corn ear stage, neither manual spraying nor drone spraying can effectively prevent and control the damage of the fall armyworm on corn ears. Moreover, due to the drift of fog droplets in traditional spraying, a great waste of pesticides is caused, and it also has a certain impact on beneficial organisms such as bees. In addition, in South China, especially in Guangdong Province, the rainfall is large. After the pesticides are applied, they are washed away by rainwater, and the amount that can actually be used for pest control is very small. Therefore, there is an urgent need for a pesticide slow-release agent with directional release and rainwater washing resistance for the prevention and control of diseases and pests on corn ears. Summary of the Invention

[0004] The purpose of the present invention is to overcome the technical problem in the prior art that spraying chemical pesticides on plants is easily washed away by rainwater and cannot really play a role in preventing and controlling pests, and to provide an annular pesticide slow-release agent. The annular pesticide slow-release agent is elastic, and when it is tied to a plant, it can slowly release insecticidal active ingredients under humid environments or rain leaching conditions, and has a good prevention and control effect on diseases such as corn ear rot and pests such as the fall armyworm, safeguarding the safety of food production.

[0005] To achieve the above purpose, the present invention adopts the following technical solutions:

[0006] An annular pesticide slow-release agent, which includes an elastic ring. The elastic ring includes the following raw material components by weight percentage:

[0007] Pesticide active ingredient 0.1% - 2.0%, organic solvent 1% - 10.0%, slow-release material 2.15% - 6.7%, plant essential oil 5% - 20.0%, emulsifier 0.1% - 0.5%, organic acid 0.01% - 0.05%, and the balance is water;

[0008] The sustained-release material includes chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate, and calcium chloride.

[0009] The annular pesticide sustained-release agent of the present invention uses chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate, and calcium chloride as the sustained-release material, which can form a three-dimensional network space structure to surround the pesticide active ingredient. After being made into an elastic ring, it is both a solid ring and elastic, and can be directly sleeved and tied on the plant tree. Under humid environments or rain leaching conditions, the pesticide active ingredient is slowly released. At the same time, through experiments, it has also been proved that it has good control effects on diseases such as maize ear rot and pests such as Spodoptera frugiperda. The annular pesticide sustained-release agent of the present invention solves the harm of pests such as Spodoptera frugiperda on plant trees, can significantly improve the insecticidal control effect, reduce the amount of pesticides used, extend the pesticide prevention and control time, and thus safeguard the safety of food production.

[0010] Further, the pesticide active ingredient includes an insecticide or a fungicide or a mixture of the above two; the insecticide is one or a mixture of two or more of chlorantraniliprole, emamectin benzoate, indoxacarb, tetrachlorantraniliprole, beta-cyhalothrin, cyfluthrin, fenpropathrin, deltamethrin, acephate, lufenuron, chlorfenapyr, and dimehypo; the fungicide is one or a mixture of two or more of penconazole, tebuconazole, hymexazol, jinggangmycin, thiabendazole, thiophanate-methyl, difenoconazole, and carboxin.

[0011] Further, the organic solvent is one or a mixture of two or more of acetone, dimethyl sulfoxide, N,N-dimethylacetamide, ethanol, ethylene glycol, ethyl acetate, toluene, xylene, cyclohexanone, hexane, petroleum ether, and ether.

[0012] Further, calculated by percentage of the raw materials, the sustained-release material includes 0.05 - 0.3% of chitosan, 1% - 3% of sodium alginate, 0.05 - 0.3% of carboxymethyl chitosan, 0.05 - 0.1% of sodium tripolyphosphate, and 1% - 3% of calcium chloride.

[0013] Further, the plant essential oil is one or a mixture of two or more of Sabina vulgaris Ant. essential oil, Artemisia scoparia Waldst. & Kit. essential oil, Acorus calamus L. essential oil, bergamot oil, birch tar, lavender oil, thyme oil, coconut oil, peppermint oil, pyrethrum, cardamom oil, citronella oil, clove oil, cinnamon oil, eucalyptus oil, neroli oil, camphor, Artemisia scoparia essential oil, wintergreen oil, Ageratina adenophora essential oil, wintergreen oil, tea tree oil, Litsea cubeba essential oil, patchouli oil, mentha spicata oil, lavender oil, cassia bark oil.

[0014] Further, the emulsifier is one or a mixture of two or more of Tween 20, Tween 40, Tween 60, Tween 80, Span 20, Span 40, Span 60, and Span 80; the organic acid is acetic acid.

[0015] Further, the ring width of the elastic ring is 2 cm to 10 cm.

[0016] The present invention also provides a preparation method of the annular pesticide slow-release agent, and the preparation method includes the following steps:

[0017] Raw material preparation: Prepare the raw materials in the formula amount;

[0018] Dissolve the pesticide active ingredient: Dissolve the pesticide active ingredient in an organic solvent to obtain a pesticide active ingredient solution;

[0019] Dissolve chitosan: Dissolve chitosan in an organic acid to obtain a chitosan solution;

[0020] Mixing and emulsifying: Mix the pesticide active ingredient solution and the chitosan solution, and add an emulsifier to obtain an emulsified mixture;

[0021] Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture;

[0022] Stir the emulsified mixture and the first mixture evenly to obtain a second mixture;

[0023] Add sodium alginate to water and stir evenly to obtain a sodium alginate solution;

[0024] Add the sodium alginate solution to the second mixture, and add plant essential oil, and stir evenly to obtain a third mixture;

[0025] Add the third mixture into the ring forming groove of the mold, dissolve calcium chloride in water to make a calcium chloride solution, add the calcium chloride solution into the ring forming groove to carry out a cross-linking reaction with the third mixture, demold after curing, and obtain the annular pesticide slow-release agent.

[0026] Further, the time of the cross-linking reaction is 30 to 60 min.

[0027] The present invention also provides an application of the annular pesticide slow-release agent, and the annular pesticide slow-release agent is used to control pests on plant trees. The specific method for applying the pest control is: Tie the annular pesticide slow-release agent to the plant tree.

[0028] Compared with the prior art, the beneficial effects of the present invention are:

[0029] (1) The annular pesticide slow-release agent of the present invention uses chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate, and calcium chloride as slow-release materials, which can form a three-dimensional network space structure to surround the pesticide active ingredient. After being made into an elastic ring, it is both a solid ring and elastic, and can be sleeved and tied on plant tree trunks. Under humid environments or rain leaching conditions, the pesticide active ingredients are slowly released, having good control effects on diseases such as maize ear rot and pests such as Spodoptera frugiperda, significantly improving the insecticidal control effect, reducing the amount of pesticides used, and extending the pesticide prevention and control time, thereby safeguarding food production safety.

[0030] (2) The annular pesticide slow-release agent of the present invention not only has a simple preparation process and low cost; at the same time, the annular pesticide slow-release agent is easy to operate during application, does not require pesticide application equipment, and can be simply sleeved on the target fruit, saving labor and time.

[0031] (3) The annular pesticide slow-release agent of the present invention can act precisely on the control target, perform fixed-point and precise prevention and control on the parts to be controlled, and has less impact on non-target organisms, effectively improving the utilization rate of pesticides.

[0032] (4) It is applicable to areas with large precipitation in South China and can be used all-weather, even on rainy days and windy days.

[0033] (5) Environmentally safe. Compared with other pesticide formulations, the annular pesticide slow-release agent of the present invention reduces the usage amount of organic solvents during the preparation process, reducing residues in the environment. BRIEF DESCRIPTION OF THE DRAWINGS

[0034] Figure 1 It is a schematic structural diagram of the mold used in the preparation method of an annular pesticide slow-release agent of the present invention;

[0035] Figure 2 It is a schematic diagram of the usage state of an annular pesticide slow-release agent of the present invention applied to a maize ear. DETAILED DESCRIPTION OF THE INVENTION

[0036] The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the accompanying drawings in the embodiments of the present invention. Obviously, the described embodiments are only a part of the embodiments of the present invention, rather than all of the embodiments. All other embodiments obtained by those of ordinary skill in the art without creative efforts shall fall within the protection scope of the present invention.

[0037] Example 1

[0038] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: chlorantraniliprole 0.1%, dimethyl sulfoxide 2.5%, slow-release material 4.25%, citronella oil 10.0%, Tween 80 0.4%, acetic acid 0.02%, and the balance is water.

[0039] Among them, the sustained-release material includes 0.1% chitosan, 2% sodium alginate, 0.1% carboxymethyl chitosan, 0.05% sodium tripolyphosphate, and 2% calcium chloride by weight percentage of the total raw materials.

[0040] This embodiment also provides a preparation method of the annular pesticide sustained-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is provided on the substrate 10.

[0041] The specific steps of the preparation method of the annular pesticide sustained-release agent are as follows:

[0042] (1) Raw material preparation: Accurately weigh the following raw materials by weight percentage, including: 0.1% chlorantraniliprole, 2.5% dimethyl sulfoxide, 4.25% sustained-release material, 10.0% citronella oil, 0.4% Tween 80, 0.02% acetic acid, and the balance is water. Among them, the sustained-release material includes 0.1% chitosan, 2% sodium alginate, 0.1% carboxymethyl chitosan, 0.05% sodium tripolyphosphate, and 2% calcium chloride by weight percentage of the total raw materials.

[0043] (2) Dissolve chlorantraniliprole in dimethyl sulfoxide to obtain a chlorantraniliprole solution, and stir magnetically for 1 h - 2 h;

[0044] (3) Add chitosan to acetic acid solution to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0045] (4) Mix the chlorantraniliprole solution and the chitosan solution and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0046] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0047] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0048] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and mechanically stir for 3 h - 5 h;

[0049] (8) Mix the sodium alginate solution and the second mixture and add citronella oil, and mechanically stir for 2 h - 4 h to obtain a third mixture;

[0050] (9) Add the third mixture into the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to make a calcium chloride solution, and add the calcium chloride solution into the annular forming groove 11 to crosslink and react with the third mixture for 30 min - 1 h, then wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0051] In this embodiment, the annular pesticide slow-release agent contains 0.18% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is chlorantraniliprole.

[0052] In this embodiment, the application of the annular pesticide slow-release agent is also provided. The annular pesticide slow-release agent prepared in this embodiment is used to control pests on plants. As Figure 2 shown, the annular pesticide slow-release agent 20 prepared in this embodiment is tied to the corn ear 30 to control pests and diseases on the corn ear.

[0053] Example 2

[0054] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: indoxacarb 0.2%, acetone 6%, slow-release material 2.35%, wintergreen oil 5%, Tween 80 0.2%, acetic acid 0.03%, and the balance is water.

[0055] Among them, the slow-release material includes 0.15% of chitosan, 1% of sodium alginate, 0.15% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate, and 1% of calcium chloride by weight percentage of the total raw materials.

[0056] This embodiment also provides a preparation method of the annular pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is formed on the substrate 10.

[0057] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0058] (1) Raw material preparation: Accurately weigh the following raw materials by weight percentage, including: indoxacarb 0.2%, acetone 5%, slow-release material 2.35%, wintergreen oil 5%, Tween 80 0.2%, acetic acid 0.03%, and the balance is water. Among them, the slow-release material includes 0.15% of chitosan, 1% of sodium alginate, 0.15% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate, and 1% of calcium chloride by weight percentage of the total raw materials.

[0059] (2) Dissolve indoxacarb in acetone to obtain an indoxacarb solution, and stir magnetically for 1 h - 2 h;

[0060] (3) Dissolve chitosan in acetic acid solution to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0061] (4) Mix the indoxacarb solution and the chitosan solution, and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0062] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0063] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0064] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h;

[0065] (8) Mix the sodium alginate solution and the second mixture, and add wintergreen oil, and stir mechanically for 2 h - 4 h to obtain a third mixture;

[0066] (9) Add the third mixture to the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to prepare a calcium chloride solution, and add the calcium chloride solution to the annular forming groove 11 to carry out a cross-linking reaction with the third mixture for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0067] In this embodiment, the annular pesticide slow-release agent contains 0.37% of a pesticide active ingredient by weight percentage, and the pesticide active ingredient is indoxacarb.

[0068] Example 3

[0069] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: 0.5% of tetrachlorantraniliprole, 2% of dimethyl sulfoxide, 4.0% of a slow-release material, 15% of litsea cubeba oil, 0.5% of Tween 80 and Span 80 (2:1), 0.05% of acetic acid, and the balance is water.

[0070] Among them, the slow-release material includes 0.2% of chitosan, 1.5% of sodium alginate, 0.2% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate, and 2% of calcium chloride by weight percentage of the total raw materials.

[0071] This embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is formed on the substrate 10.

[0072] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0073] (1) Raw material preparation: Accurately weigh the following raw materials by weight percentage, including: tetrachlorantraniliprole 0.5%, dimethyl sulfoxide 2%, slow-release material 4.0%, litsea cubeba oil 15%, Tween 80 and Span 80 (2:1) 0.5%, acetic acid 0.05%, and the balance is water. Among them, the slow-release material includes chitosan 0.2%, sodium alginate 1.5%, carboxymethyl chitosan 0.2%, sodium tripolyphosphate 0.1%, and calcium chloride 2% by weight percentage of the total raw materials.

[0074] (2) Dissolve tetrachlorantraniliprole in dimethyl sulfoxide to obtain a tetrachlorantraniliprole solution, and stir magnetically for 1 h - 2 h;

[0075] (3) Add chitosan to acetic acid solution to dissolve and obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0076] (4) Mix the tetrachlorantraniliprole solution and the chitosan solution, and add Tween 80 and Span 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0077] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0078] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0079] (7) Add water to sodium alginate and stir mechanically to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h;

[0080] (8) Mix the sodium alginate solution and the second mixture, and add litsea cubeba oil, and stir mechanically for 2 h - 4 h to obtain a third mixture;

[0081] (9) Add the third mixture to the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to make a calcium chloride solution, and add the calcium chloride solution to the annular forming groove 11 to crosslink and react with the third mixture for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0082] In this embodiment, the annular pesticide slow-release agent contains 0.95% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is tetrachlorantraniliprole.

[0083] Example 4

[0084] A ring-shaped pesticide slow-release agent is prepared from the following raw materials by weight percentage: lambda-cyhalothrin 0.2%, ethyl acetate 2.5%, slow-release material 4.6%, cinnamon oil 12.5%, Tween 80 0.3%, acetic acid 0.04%, and the balance is water. Among them, the slow-release material includes chitosan 0.2%, sodium alginate 2%, carboxymethyl chitosan 0.3%, sodium tripolyphosphate 0.1%, and calcium chloride 2% by weight percentage of the total raw materials.

[0085] This embodiment also provides a preparation method of the ring-shaped pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and a ring-shaped forming groove 11 is formed on the substrate 10.

[0086] The specific steps of the preparation method of the ring-shaped pesticide slow-release agent are as follows:

[0087] (1) Accurately weigh various raw materials: lambda-cyhalothrin 0.2%, ethyl acetate 2.5%, slow-release material 4.6%, cinnamon oil 12.5%, Tween 80 0.3%, acetic acid 0.04%, and the balance is water.

[0088] (2) Dissolve lambda-cyhalothrin in ethyl acetate to obtain a lambda-cyhalothrin solution, and stir magnetically for 1 h - 2 h;

[0089] (3) Add chitosan to acetic acid water to dissolve to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0090] (4) Mix the chitosan solution and the lambda-cyhalothrin solution and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0091] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0092] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0093] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and mechanically stir for 3 h - 5 h;

[0094] (8) Mix the sodium alginate solution and the second mixture and add cinnamon oil, and mechanically stir for 2 h - 4 h to obtain a third mixture;

[0095] (9) Add the third mixture to the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to make a calcium chloride solution, and add the calcium chloride solution to the annular forming groove 11 to crosslink and react with the third mixture for 30 min - 1 h, then wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0096] In this embodiment, the annular pesticide slow-release agent contains 0.36% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is lambda-cyhalothrin.

[0097] Example 5

[0098] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: deltamethrin 0.1%, xylene 2.5%, slow-release material 5.35%, clove oil 7.5%, Tween 80 and Tween 60 (1:1) 0.3%, acetic acid 0.05%, and the balance is water.

[0099] Among them, the slow-release material includes 0.1% of chitosan, 3% of sodium alginate, 0.2% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate, and 2% of calcium chloride by weight percentage of the total raw materials.

[0100] This embodiment also provides a preparation method of the annular pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is formed on the substrate 10.

[0101] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0102] (1) Accurately weigh various raw materials: deltamethrin 0.1%, xylene 2.5%, slow-release material 5.35%, clove oil 7.5%, Tween 80 and Tween 60 (1:1) 0.3%, acetic acid 0.05%, and the balance is water.

[0103] (2) Dissolve deltamethrin in xylene to obtain a deltamethrin solution, and stir magnetically for 1 h - 2 h;

[0104] (3) Add chitosan to acetic acid solution to dissolve and obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0105] (4) Mix the deltamethrin solution and the chitosan solution and add Tween 80 and Tween 60 (1:1) to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0106] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0107] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and magnetically stir for 1 h - 2 h;

[0108] (7) Add water to sodium alginate and mechanically stir to obtain a sodium alginate solution, and mechanically stir for 3 h - 5 h;

[0109] (8) Mix the sodium alginate solution and the second mixture and add clove oil, and mechanically stir for 2 h - 4 h to obtain a third mixture;

[0110] (9) Add the third mixture to an annular mold through a peristaltic pump, add a calcium chloride solution, crosslink for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0111] The annular pesticide slow-release agent obtained in this embodiment is an annular pesticide slow-release agent containing 0.17% of deltamethrin.

[0112] Example 6

[0113] An annular pesticide slow-release agent, comprising the following raw materials by weight percentage: 0.5% of penconazole, 1.0% of toluene, 4.5% of slow-release material, 10% of calamus essential oil, 0.4% of Tween 80, 0.01% of acetic acid, and the balance is water.

[0114] Among them, the slow-release material includes 0.2% of chitosan, 2% of sodium alginate, 0.2% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate, and 2% of calcium chloride by weight percentage of the raw materials.

[0115] This embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is provided on the substrate 10.

[0116] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0117] (1) Accurately weigh various raw materials: 0.5% of penconazole, 1.0% of toluene, 4.5% of slow-release material, 10% of calamus essential oil, 0.4% of Tween 80, 0.01% of acetic acid, and the balance is water.

[0118] (2) Dissolve penconazole in toluene to obtain a penconazole solution, and magnetically stir for 1 h - 2 h;

[0119] (3) Add chitosan to acetic acid solution to obtain a chitosan solution, and magnetically stir for 1 h - 2 h;

[0120] (4) Mix the penconazole solution and the chitosan solution and add Tween 80 to obtain an emulsified mixture, and magnetically stir for 1 h - 2 h;

[0121] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixed solution, and stir magnetically for 1 h - 2 h;

[0122] (6) Mix the emulsified mixed solution and the first mixed solution to obtain a second mixed solution, and stir magnetically for 1 h - 2 h;

[0123] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h;

[0124] (8) Mix the sodium alginate solution and the second mixed solution and add calamus essential oil, and stir mechanically for 2 h - 4 h to obtain a third mixed solution;

[0125] (9) Add the third mixed solution into the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to make a calcium chloride solution, and add the calcium chloride solution into the annular forming groove 11 to carry out a cross-linking reaction with the third mixed solution for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0126] The annular pesticide slow-release agent prepared in this embodiment is an annular pesticide slow-release agent of penconazole with a pesticide active ingredient content of 0.8%.

[0127] Example 7

[0128] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: difenoconazole 0.5%, acetone 1.0%, slow-release material 4.9%, bergamot oil 6%, Tween 80 and Span 80 (3:1) 0.5%, acetic acid 0.05%, and the balance is water.

[0129] Among them, the slow-release material includes 0.4% of chitosan, 2% of sodium alginate, 0.4% of carboxymethyl chitosan, 0.1% of sodium tripolyphosphate, and 2% of calcium chloride by weight percentage of the total raw materials.

[0130] This embodiment also provides a preparation method of the annular pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is opened on the substrate 10.

[0131] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0132] (1) Accurately weigh various raw materials: difenoconazole 0.5%, acetone 1.0%, slow-release material 4.9%, bergamot oil 6%, Tween 80 and Span 80 (3:1) 0.5%, acetic acid 0.05%, and the balance is water.

[0133] (2) Dissolve difenoconazole in toluene to obtain a difenoconazole solution, and stir magnetically for 1 h - 2 h;

[0134] (3) Dissolve chitosan in acetic acid solution to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0135] (4) Mix the difenoconazole solution and the chitosan solution, and add Tween 80 and Span 80 (3:1) to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0136] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0137] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0138] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h;

[0139] (8) Mix the sodium alginate solution and the second mixture, and add bergamot oil, and stir mechanically for 2 h - 4 h to obtain a third mixture;

[0140] (9) Add the third mixture to the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to prepare a calcium chloride solution. Add the calcium chloride solution to the annular forming groove 11 to carry out a cross-linking reaction with the third mixture for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0141] In this embodiment, the annular pesticide slow-release agent contains 1.60% of a pesticide active agent by weight percentage, and the pesticide active agent is difenoconazole.

[0142] Example 8

[0143] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: thiophanate-methyl 1%, acetone 5%, slow-release material 2.75%, thymol 5%, Tween 80 0.5%, acetic acid 0.04%, and the balance is water.

[0144] Among them, the slow-release material includes 0.1% of chitosan, 1.5% of sodium alginate, 0.1% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate, and 1% of calcium chloride by weight percentage of the total raw materials.

[0145] This embodiment also provides a preparation method of the annular pesticide slow-release agent, and the structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is formed on the substrate 10.

[0146] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0147] (1) Weigh accurately various raw materials: 1% of thiophanate-methyl, 5% of acetone, 2.75% of slow-release material, 5% of thymol, 0.5% of Tween 80, 0.04% of acetic acid, and the balance is water.

[0148] (2) Dissolve thiophanate-methyl in dimethyl sulfoxide to obtain a thiophanate-methyl solution, and stir magnetically for 1 h - 2 h.

[0149] (3) Add chitosan to acetic acid solution to dissolve and obtain a chitosan solution, and stir magnetically for 1 h - 2 h.

[0150] (4) Mix the thiophanate-methyl solution and the chitosan solution, and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h.

[0151] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h.

[0152] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h.

[0153] (7) Stir sodium alginate mechanically in water to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h.

[0154] (8) Mix the sodium alginate solution and the second mixture, and add thymol, and stir mechanically for 2 h - 4 h to obtain a third mixture.

[0155] (9) Add the third mixture to the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to make a calcium chloride solution, and add the calcium chloride solution to the annular forming groove 11 to carry out a cross-linking reaction with the third mixture for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0156] In this embodiment, the annular pesticide slow-release agent contains 1.93% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is thiophanate-methyl.

[0157] Example 9

[0158] An annular pesticide slow-release agent is prepared from the following raw materials by weight percentage: 0.2% of jinggangmycin, 2% of dimethyl sulfoxide, 3.65% of slow-release material, 5% of thymol, 0.5% of Tween 80, 0.01% of acetic acid, and the balance is water.

[0159] Among them, the slow-release material includes 0.05% of chitosan, 1.5% of sodium alginate, 0.05% of carboxymethyl chitosan, 0.05% of sodium tripolyphosphate, and 2% of calcium chloride by weight percentage of the total raw materials.

[0160] This embodiment also provides a preparation method of the annular pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and an annular forming groove 11 is formed on the substrate 10.

[0161] The specific steps of the preparation method of the annular pesticide slow-release agent are as follows:

[0162] (1) Accurately weigh various raw materials: 0.2% of jinggangmycin, 2% of dimethyl sulfoxide, 3.65% of slow-release material, 5% of thymol, 0.5% of Tween 80, 0.01% of acetic acid, and the balance is water.

[0163] (2) Dissolve jinggangmycin in dimethyl sulfoxide to obtain a jinggangmycin solution, and stir magnetically for 1 h - 2 h;

[0164] (3) Add chitosan to acetic acid solution to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0165] (4) Mix the jinggangmycin solution and the chitosan solution, and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0166] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0167] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0168] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and stir mechanically for 3 h - 5 h;

[0169] (8) Mix the sodium alginate solution and the second mixture, and add thymol, and stir mechanically for 2 h - 4 h to obtain a third mixture;

[0170] (9) Add the third mixture into the annular forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to prepare a calcium chloride solution, and add the calcium chloride solution into the annular forming groove 11 to carry out a cross-linking reaction with the third mixture for 30 min - 1 h, and wash with deionized water to obtain an annular pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0171] In this embodiment, the annular pesticide slow-release agent contains 0.34% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is jinggangmycin.

[0172] Example 10

[0173] A ring-shaped pesticide slow-release agent is prepared from the following raw materials by weight percentage: tebuconazole 0.2%, toluene 4%, slow-release material 3.3%, Artemisia scoparia essential oil 5%, Tween 80 0.5%, acetic acid 0.02%, and the balance is water.

[0174] Among them, the slow-release material includes chitosan 0.1%, sodium alginate 1%, carboxymethyl chitosan 0.1%, sodium tripolyphosphate 0.1%, and calcium chloride 2% by weight percentage of the total raw materials.

[0175] This embodiment also provides a preparation method of the ring-shaped pesticide slow-release agent. The structure of the mold used in the preparation method is as Figure 1 shown. The mold includes a substrate 10, and a ring-shaped forming groove 11 is formed on the substrate 10.

[0176] The specific steps of the preparation method of the ring-shaped pesticide slow-release agent are as follows:

[0177] (1) Accurately weigh various raw materials: tebuconazole 0.2%, toluene 4%, slow-release material 3.3%, Artemisia scoparia essential oil 5%, Tween 80 0.5%, acetic acid 0.02%, and the balance is water.

[0178] (2) Dissolve tebuconazole in dimethyl sulfoxide to obtain a tebuconazole solution, and stir magnetically for 1 h - 2 h;

[0179] (3) Add chitosan to acetic acid water to dissolve to obtain a chitosan solution, and stir magnetically for 1 h - 2 h;

[0180] (4) Mix the tebuconazole solution and the chitosan solution and add Tween 80 to obtain an emulsified mixture, and stir magnetically for 1 h - 2 h;

[0181] (5) Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture, and stir magnetically for 1 h - 2 h;

[0182] (6) Mix the emulsified mixture and the first mixture to obtain a second mixture, and stir magnetically for 1 h - 2 h;

[0183] (7) Mechanically stir sodium alginate in water to obtain a sodium alginate solution, and mechanically stir for 3 h - 5 h;

[0184] (8) Mix the sodium alginate solution and the second mixture and add thymol, and mechanically stir for 2 h - 4 h to obtain a third mixture;

[0185] (9) Add the third mixture to the ring-shaped forming groove 11 of the mold through a peristaltic pump. Dissolve calcium chloride in water to prepare a calcium chloride solution, and add the calcium chloride solution to the ring-shaped forming groove 11 to carry out a cross-linking reaction with the third mixture for 30 min - 1 h, and wash with deionized water to obtain a ring-shaped pesticide slow-release agent with a diameter of 2 cm - 10 cm.

[0186] In this embodiment, the annular pesticide slow-release agent contains 0.36% of pesticide active ingredient by weight percentage, and the pesticide active ingredient is tebuconazole.

[0187] Field trial 1

[0188] The annular pesticide slow-release agents prepared in Examples 1-5 were used to control a test corn field with Spodoptera frugiperda ear pests, together with a certain brand of chlorantraniliprole suspension, tetrachlorantraniliprole and chlorfenapyr suspension on the market.

[0189] Application method:

[0190] Apply the medicine once. Spray the three preparations of chlorantraniliprole suspension, tetrachlorantraniliprole and chlorfenapyr suspension, and manually put the ring of the annular pesticide slow-release agent around the corn ear.

[0191] Investigation method:

[0192] After each plot was delimited, the damage situation of the corn ears at each point was investigated by the "Z"-shaped five-point sampling method. For each treatment, 3 plots were investigated, 20 plants were randomly investigated at each point, and a total of 100 plants were investigated in each plot. If live Spodoptera frugiperda insects were found in the corn ears, it was recorded as a damaged plant. Record the number of damaged plants in each corn field and the number of live insects in the corn ears, and calculate the efficacy of the medicine according to the standard of GB / T17980.6-2000:

[0193]

[0194] In the formula: CK—the damaged ear rate of the blank control area; PT—the damaged ear rate of the medicament treatment area.

[0195]

[0196] In the formula: CK1—the number of live insects on the ears in the blank control treatment area; PT1—the number of live insects on the ears in the medicament treatment area.

[0197] The ear protection control effect is as follows in Table 1:

[0198]

[0199]

[0200] As can be seen from Table 1, compared with the control treatment medicament, the annular pesticide slow-release agents prepared in Examples 1-5 have significantly improved the ear protection control effect on corn ears.

[0201] The insecticidal control effect is as follows in Table 2:

[0202]

[0203] As can be seen from Table 2, compared with the control treatment agent, the annular pesticide sustained-release agents prepared in Examples 1-5 have significantly improved the control effect on Spodoptera frugiperda.

[0204] Field experiment 2

[0205] The annular pesticide sustained-release agents prepared in Examples 6-10 were used to control the experimental corn fields with maize ear rot together with a 10% penconazole emulsifiable concentrate, a 36% thiophanate-methyl suspension concentrate, and a 5% jinggangmycin aqueous solution of a certain brand on the market.

[0206] Application method:

[0207] Apply the medicine once. The three preparations of 10% penconazole emulsifiable concentrate, 36% thiophanate-methyl suspension concentrate, and 5% jinggangmycin aqueous solution were used for spray treatment, and the annular pesticide sustained-release agent was manually put the ring on the corn ear.

[0208] Investigation method:

[0209] After each plot was delimited, the total number of ears, the number of diseased ears, and the disease level in each plot were investigated, the disease index was calculated, and the control effect was calculated based on the disease index of each agent treatment and the disease index of the blank control group.

[0210] Disease grading standard: Grade 0, the incidence rate is 0; Grade 1, the diseased area accounts for less than 1% of the total area of the ear; Grade 3, the diseased area accounts for 2% - 10% of the total area of the ear; Grade 5, the diseased area accounts for 11% - 25% of the total area of the ear; Grade 7, the diseased area accounts for 26% - 50% of the total area of the ear; Grade 9, the diseased area accounts for 51% - 100% of the total area of the ear.

[0211] Pharmacodynamic calculation method:

[0212] Disease index = Z (number of diseased ears at each level x representative value at each level) / (total number of ears investigated x representative value of the highest level) x 100;

[0213] Control effect (%) = [1 - (T - To) / (ck - cko)] × 100.

[0214] T and To are the final disease conditions and the initial disease conditions in the control area respectively; ck and cko are the final disease conditions and the initial disease conditions in the control area respectively.

[0215] The control effects are as shown in Table 3 below:

[0216]

[0217]

[0218] As can be seen from Table 3, compared with the control treatment agent, the annular pesticide sustained-release agents prepared in Examples 6-10 have significantly improved the control effect on maize ear rot.

[0219] In summary, for the annular pesticide slow-release agent of the present invention, by using natural polymer materials as slow-release agents and plant essential oils as repellents or insecticidal and fungicidal agents, the problems in the prior art that less pesticide reaches the ear part, resulting in great waste and difficulty in controlling pests and diseases on the ear part are solved. The preparation process is simple and the cost is low. At the same time, the annular pesticide slow-release agent is easy to operate during application, effectively improving the utilization rate of pesticides.

[0220] The above are the preferred embodiments of the present invention, but the present invention should not be limited to the embodiments and the content disclosed in the drawings. Therefore, all equivalent or modified implementations completed without departing from the spirit disclosed by the present invention fall within the protection scope of the present invention.

Claims

1. A ring-shaped pesticide sustained-release agent for preventing and controlling Spodoptera frugiperda and maize ear rot, characterized in that, it is an elastic ring, and the elastic ring is tied to plants to control pests. The elastic ring comprises the following raw material components by weight percentage: Pesticide active agent 0.1 - 2.0%, organic solvent 1 - 10.0%, sustained-release material 2.15 - 6.7%, plant essential oil 5 - 20.0%, emulsifier 0.1 - 0.5%, organic acid 0.01 - 0.05%, and the balance is water; The sustained-release material is chitosan, sodium alginate, carboxymethyl chitosan, sodium tripolyphosphate and calcium chloride; The pesticide active agent is an insecticide or a fungicide; the insecticide is one of chlorantraniliprole, indoxacarb, tetrachlorantraniliprole, lambda-cyhalothrin, deltamethrin; the fungicide is one of penconazole, tebuconazole, thiophanate-methyl, difenoconazole; The organic solvent is one or a mixture of two or more of acetone, dimethyl sulfoxide, N, N-dimethylacetamide, ethanol, ethylene glycol, ethyl acetate, toluene, xylene, cyclohexanone, hexane, petroleum ether and ether; By percentage of the raw materials, chitosan 0.05 - 0.3%, sodium alginate 1 - 3%, carboxymethyl chitosan 0.05 - 0.3%, sodium tripolyphosphate 0.05 - 0.1%, calcium chloride 1 - 3%; The plant essential oil is one of Artemisia scoparia essential oil, Acorus calamus essential oil, bergamot oil, thymol oil, citronella oil, clove oil, cinnamon oil, wintergreen oil, Litsea cubeba oil; The emulsifier is one or a mixture of two or more of Tween 20, Tween 40, Tween 60, Tween 80, Span 20, Span 40, Span 60, Span 80; the organic acid is acetic acid; The ring width of the elastic ring is 2 cm - 10 cm; The preparation method of the ring-shaped pesticide sustained-release agent comprises the following steps: Raw material preparation: Prepare the raw materials in the formula amount; Dissolve the pesticide active agent: Dissolve the pesticide active agent in the organic solvent to obtain a pesticide active agent solution; Dissolve chitosan: Dissolve chitosan in the organic acid to obtain a chitosan solution; Mix and emulsify: Mix the pesticide active agent solution and the chitosan solution, and add the emulsifier to obtain an emulsified mixture; Dissolve carboxymethyl chitosan and sodium tripolyphosphate in water to obtain a first mixture; Stir the emulsified mixture and the first mixture evenly to obtain a second mixture; Add sodium alginate to water and stir evenly to obtain a sodium alginate solution; Add the sodium alginate solution to the second mixture, and add the plant essential oil, and stir evenly to obtain a third mixture; Add the third mixture to the ring-shaped forming groove of the mold, dissolve calcium chloride in water to make a calcium chloride solution, add the calcium chloride solution to the ring-shaped forming groove to carry out a cross-linking reaction with the third mixture, and demold after curing to obtain the ring-shaped pesticide sustained-release agent; The time of the cross-linking reaction is 30 - 60 min.

Citation Information

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