CN116831133B - Emamectin benzoate water dispersible granule and preparation method thereof - Google Patents
Emamectin benzoate water dispersible granule and preparation method thereof Download PDFInfo
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- CN116831133B CN116831133B CN202310808457.4A CN202310808457A CN116831133B CN 116831133 B CN116831133 B CN 116831133B CN 202310808457 A CN202310808457 A CN 202310808457A CN 116831133 B CN116831133 B CN 116831133B
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- emamectin benzoate
- filler
- water dispersible
- dispersible granule
- pesticide
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- 239000004562 water dispersible granule Substances 0.000 title claims abstract description 50
- CXEGAUYXQAKHKJ-NSBHKLITSA-N emamectin B1a Chemical compound C1=C[C@H](C)[C@@H]([C@@H](C)CC)O[C@]11O[C@H](C\C=C(C)\[C@@H](O[C@@H]2O[C@@H](C)[C@H](O[C@@H]3O[C@@H](C)[C@H](NC)[C@@H](OC)C3)[C@@H](OC)C2)[C@@H](C)\C=C\C=C/2[C@]3([C@H](C(=O)O4)C=C(C)[C@@H](O)[C@H]3OC\2)O)C[C@H]4C1 CXEGAUYXQAKHKJ-NSBHKLITSA-N 0.000 title claims abstract 9
- 238000002360 preparation method Methods 0.000 title abstract description 19
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- FYGDTMLNYKFZSV-URKRLVJHSA-N (2s,3r,4s,5s,6r)-2-[(2r,4r,5r,6s)-4,5-dihydroxy-2-(hydroxymethyl)-6-[(2r,4r,5r,6s)-4,5,6-trihydroxy-2-(hydroxymethyl)oxan-3-yl]oxyoxan-3-yl]oxy-6-(hydroxymethyl)oxane-3,4,5-triol Chemical compound O[C@@H]1[C@@H](O)[C@H](O)[C@@H](CO)O[C@H]1OC1[C@@H](CO)O[C@@H](OC2[C@H](O[C@H](O)[C@H](O)[C@H]2O)CO)[C@H](O)[C@H]1O FYGDTMLNYKFZSV-URKRLVJHSA-N 0.000 claims abstract description 17
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- QEKATQBVVAZOAY-UHFFFAOYSA-M sodium;4-propan-2-ylbenzenesulfonate Chemical compound [Na+].CC(C)C1=CC=C(S([O-])(=O)=O)C=C1 QEKATQBVVAZOAY-UHFFFAOYSA-M 0.000 claims description 3
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Classifications
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/12—Powders or granules
- A01N25/14—Powders or granules wettable
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/24—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests containing ingredients to enhance the sticking of the active ingredients
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/30—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests characterised by the surfactants
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
-
- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01P—BIOCIDAL, PEST REPELLANT, PEST ATTRACTANT OR PLANT GROWTH REGULATORY ACTIVITY OF CHEMICAL COMPOUNDS OR PREPARATIONS
- A01P7/00—Arthropodicides
- A01P7/04—Insecticides
Abstract
The invention discloses an emamectin benzoate water dispersible granule and a preparation method thereof, wherein the emamectin benzoate water dispersible granule comprises the following components: emamectin benzoate, defoamer, wetting agent, dispersant, surfactant, binder and filler; the invention uses yeast beta-glucan to react with allyl glycidyl ether, the obtained modified compound is successfully grafted with tetramethyl divinyl disilazane to obtain a filler, and pesticide molecules are encapsulated by the filler to form the emamectin benzoate water dispersible granule. Compared with the prior art, the emamectin benzoate water dispersible granule prepared by the invention has the advantages of controlled release, ultraviolet resistance and environmental friendliness, and has better control effect on rice stem borers.
Description
Technical Field
The invention relates to the technical field of pesticides, in particular to an emamectin benzoate water dispersible granule and a preparation method thereof.
Background
Emamectin benzoate, commonly referred to as emamectin benzoate, is a subverted semisynthetic antibiotic pesticide. The production process of the pesticide refers to the structure of abamectin and reforms the abamectin. Compared with avermectin, the emamectin benzoate has reduced toxicity by at least 66.7%, however, the biological activity is rapidly increased, and the improvement range is about 10 to 1000 times. The emamectin benzoate is mainly characterized by comprising the following components: high-efficiency insecticidal, broad-spectrum application, low toxicity, no residue, no cross resistance and the like, and is widely considered as the best choice for replacing high-toxicity pesticides. Emamectin benzoate pesticides have been widely adopted in some developed countries and play an important role in agricultural production.
The principle of action of emamectin benzoate is to cause a large amount of chloride ions to enter nerve cells by strengthening neurotransmitter activity, thereby making these cells unable to function properly. This process can cause the pest to stop feeding within hours and go into a paralytic state, ultimately leading to its death. As a compound, emamectin benzoate acts mainly through stomach toxicity and also has a contact killing function.
The emamectin benzoate has remarkable insecticidal effect on many types of pests, particularly lepidoptera, diptera, homoptera, coleoptera and thysanoptera pests, and the effect is particularly remarkable. For example, red leaf rollers, tobacco budworms, beet armyworms, dry land spodoptera, cabbage loopers, tobacco loopers, plutella xylostella, citrus leaf miners, prodenia litura, tomato loopers, potato ladybug, cabbage borers, rice leaf rollers, chilo suppressalis, tryporyza incertulas, cotton bollworms, pear psyllids, peach fruit moths, aphids and other pests all exhibit extremely high sensitivity after contacting emamectin benzoate.
In addition, emamectin also exhibits excellent resistance to mite pests such as citrus red spider, apple red spider, cotton red spider, apple spider mite, and the like. The broad spectrum of emamectin benzoate and its resistance to pests is a major advantage, and emamectin benzoate is still effective against pests that have developed resistance to other pesticides. Therefore, the application field of emamectin benzoate pesticides is expanding in China.
However, the main emamectin benzoate formulations in China still mainly adopt the form of emulsifiable concentrates and microemulsions at present. These formulations contain large amounts of organic solvents such as toluene, xylene and methanol, which can have adverse effects on human health and the environment. In addition, as the price of petroleum continues to rise, the cost of these petroleum-based raw materials continues to increase. Meanwhile, the liquid form of the emulsifiable concentrate and the microemulsion preparation brings certain challenges in the links of packaging, storage, transportation and the like. Therefore, in order to solve these problems, the search and development of novel formulations to replace emulsifiable concentrates and microemulsion formulations has become an important development direction in the field of pesticide development. Due to the continuous development of green prevention and control technology, the registration use amount of granular dosage forms such as water dispersible granules is increased year by year, and the water dispersible granules become one of main development directions of future pesticide dosage forms.
The invention patent application CN107372542A discloses a 5.7% emamectin benzoate water dispersible granule, which comprises the following components: emamectin benzoate: 5.7%; dispersant KZ-008:5.6 to 6.5 percent; wetting agent KZ-016: 2-3%; lignin naphthalene sulfonate dispersant KZ-021:4 to 6 percent; biological protein KZ-088:71.1 to 73.4 percent; stabilizer KZ-031:0.5 to 1.5 percent; lactose: 1.5 to 3 percent; corn starch: 3 to 6 percent; by adding 71.3-74.6% of the biological protein KZ-088, the invention uses KZ-088 to create the production environment of emamectin benzoate, so that the biological pesticide emamectin benzoate can be more stable under a new formula, various technical indexes of the product are higher, the efficacy is more favorable, the light is more stable, and the environment is safer, more environment-friendly and more efficient. However, the water dispersible granule prepared by the invention has poor dispersibility, unsatisfactory control effect, weak ultraviolet resistance, low drug effect and environment friendliness.
Disclosure of Invention
In view of the defects of poor dispersibility, unsatisfactory prevention effect, weak ultraviolet resistance and environmental pollution of the water dispersible granule in the prior art, the technical problem to be solved by the invention is to provide the emamectin benzoate water dispersible granule which has the advantages of controlled release, good prevention effect, ultraviolet resistance and environmental friendliness and can effectively improve the pesticide utilization rate.
In order to achieve the above object, the present invention adopts the following technical scheme:
The emamectin benzoate water dispersible granule comprises the following components: emamectin benzoate, defoamer, wetting agent, dispersant, surfactant, binder and filler.
Preferably, the emamectin benzoate water dispersible granule comprises the following components in percentage by mass: 3 to 8 percent of emamectin benzoate, 0.1 to 0.5 percent of defoamer, 1 to 3 percent of wetting agent, 1 to 3 percent of dispersing agent, 0.1 to 5 percent of surfactant, 0.1 to 1 percent of binder and the balance of filler.
Preferably, the defoaming agent is at least one of polyether modified organosilane, fatty alcohol emulsified silicone oil, tributyl phosphate, sorbitan monolaurate and glycerol monoricinoleate.
Preferably, the wetting agent is at least one of alkylphenol ethoxylates, alkyl naphthalene sulfonate, acyl glutamate, fatty alcohol ethoxylates, fatty alcohol ethoxylate sulfate, fatty alcohol ethoxylate and tallow ethoxyamine salt.
Preferably, the dispersing agent is at least one of polyacrylic acid derivative, alkyl naphthalene sulfonate formaldehyde condensate, fatty acid ethylene oxide condensate, sodium polycarboxylate, alkyl polyoxyethylene ether sulfonate, alkylphenol polyoxyethylene ether phosphate, lignin sulfonate and tea saponin.
Preferably, the surfactant is at least one of fatty alcohol polyoxyethylene ether, polyvinylpyrrolidone, sodium 4-isopropylbenzene sulfonate, sodium dodecylbenzene sulfonate and sodium dodecyl sulfate.
Preferably, the binder is at least one of polyvinyl alcohol, polyethylene glycol, carboxymethyl cellulose, polyvinyl alcohol, dextrin, xanthan gum, sodium silicate, gypsum and modified starch.
The preparation method of the emamectin benzoate water dispersible granule comprises the following steps: weighing the raw materials according to the mass percentage, uniformly mixing emamectin benzoate, a defoaming agent, a wetting agent, a dispersing agent, a surfactant, a binder and a filler, carrying out superfine grinding on the mixture to below 200-400 meshes to obtain powder, and adding water, wherein the weight ratio of the water to the powder is 0.8-2: 1, granulating; and (3) drying the obtained particles at the temperature of 40-60 ℃, and screening out 50-200 meshes of particles to obtain the emamectin benzoate water dispersible granule.
Preferably, the filler is prepared by the following method, and the parts by weight are:
S1, dissolving 1-3 parts of yeast beta-glucan in 80-150 parts of water, adding 0.2-1 part of allyl glycidyl ether, stirring at room temperature at a stirring speed of 200-500 rpm for 0.5-3 hours to obtain a modified solution;
S2, dissolving 0.5-3 parts of tetramethyl divinyl disilazane in 20-50 parts of water, adding 0.1-1 part of potassium peroxodisulfate, introducing nitrogen at 60-90 ℃ at a nitrogen rate of 15-30 mL/min, and stirring for 0.5-3 hours at a stirring speed of 100-300 rpm to obtain a composite solution;
S3, dropwise adding the composite solution prepared in the step S2 into the modified solution prepared in the step S1 at 60-90 ℃ for 8-15 min, stirring for 3-10 h, stirring at 200-500 rpm, freeze-drying at-30 to-10 ℃ for 10-20 h, extracting with absolute ethyl alcohol for 40-60 h, and drying in an oven at 60-80 ℃ for 10-20 h to obtain the filler.
In the experimental process of the invention, the molecular weight of the yeast beta-glucan after the grafting reaction is increased, and the molecular weight distribution is wider. This is due to the presence of double bonds in the modified solution structure resulting from the reaction of allyl glycidyl ether with yeast beta-glucan. During the free radical initiation reaction, part of yeast beta-glucan is combined with allyl glycidyl ether molecules, and the molecular weight of the copolymer is difficult to control. Therefore, the molecular weight is increased, the molecular weight distribution range is wider, and the molecular weight is controlled within a proper range by selecting a proper addition amount.
According to the invention, yeast beta-glucan reacts with allyl glycidyl ether, the obtained modified compound is successfully grafted with tetramethyl divinyl disilazane to obtain the filler, pesticide molecules are encapsulated by the filler to form the water dispersible granule, the pesticide molecules exist in nano filler particles in an amorphous form, and compared with independent pesticide molecules, the contact angle of the water dispersible granule is smaller. The contact angle is reduced because the yeast beta-glucan and the tetramethyl divinyl disilazane reduce the surface energy of the water dispersible granule solution, and the spreadability of the water dispersible granule solution on the blade is increased, so that the liquid medicine is rapidly diffused and adhered on the blade. Therefore, the water dispersible granule pesticide effectively prevents the loss of the pesticide, promotes the proper dispersion of pesticide molecules and improves the pesticide efficiency.
The water dispersible granule can quickly release pesticide molecules in the early stage, and is mainly because part of pesticide molecules are not wrapped by nano particles and can be quickly released after being sprayed. The release rate of the encapsulated pesticide molecules tends to be stable, and the remaining amount of pesticide molecules is released over a longer period of time due to the biodegradability of the filler. The release mechanism is complex, and the drug release process can be practically divided into two phases: (1) burst release phase: initially the drug is released rapidly, free pesticide molecules deposit on the nanoparticle surface, resulting in rapid release of the pesticide molecules. (2) In the corrosion process under the acidic or alkaline condition, the filler is decomposed to form holes, and the corrosion solution enters into the filler molecules to cause corrosion of the inside of the filler molecules, so that pesticide molecules wrapped in the filler are released, but the release speed is slower due to the longer diffusion path. Therefore, the change of pH can change the stability of the filler, and control the release rate of pesticide molecules, thereby being suitable for the growth of different crops. The method is suitable for plants which need a large amount of pesticides at a certain stage, and can also be suitable for plants which need a small amount of pesticides in a long time.
The emamectin benzoate of the present invention is susceptible to ultraviolet light decomposition, so that improving its photostability is essential for its use. When ultraviolet light is continuously irradiated, the water dispersible granule without the filler continuously and rapidly decomposes the pesticide molecule water solution due to the fact that no ultraviolet barrier exists. In the embodiment 1, the filler is used as a shell material of pesticide molecular nano particles, and the yeast beta-glucan has good ultraviolet absorption performance, is an effective ultraviolet blocking barrier, and has a low degradation speed under ultraviolet irradiation, so that the filler has good ultraviolet shielding performance. Is a good pesticide slow-release reagent, in particular to a slow-release reagent of photosensitive pesticide.
An increase in the tetramethyl divinyl disilazane agent results in an increase in the grafting yield, resulting in higher hydrophobicity. The greater the amount of hydrophobic filler encapsulating the pesticide molecule, the greater the encapsulation efficiency of the sample, and therefore, more pesticide molecules can be encapsulated. However, the grafting ratio increases and the viscosity of the system increases, which is disadvantageous in that the reaction proceeds because the encapsulation efficiency becomes low. According to the invention, the proper addition amount is selected through experiments, and the obtained encapsulation efficiency is maximum.
Compared with the prior art, the invention has the beneficial effects that:
1) According to the invention, yeast beta-glucan reacts with allyl glycidyl ether, the obtained modified compound is successfully grafted with tetramethyl divinyl disilazane to obtain the filler, and pesticide molecules are encapsulated by the filler to form the water dispersible granule which has controlled release, ultraviolet resistance and environmental friendliness, so that the performance of the pesticide can be effectively improved.
2) The invention adopts scientific ingredients and a preparation method, and the prepared water dispersible granule has better dispersion adhesiveness in the medicinal process, can improve the utilization rate of medicines and enhance the insecticidal effect.
3) The invention is a low-toxicity pesticide, which can quickly paralyze, refusal to eat, slow action or immobility of pests for several hours by inhibiting the transfer of aminobutyric acid in the motor nerves of the pests, has the effects of contact killing and stomach poisoning on the pests, forms a second pest killing peak after 7 days, and has better control effect on rice stem borers when being used according to recommended dosage.
Detailed Description
The technical scheme of the present invention will be described in detail by means of specific examples, which should be explicitly set forth for illustration, but should not be construed as limiting the scope of the present invention.
The parameters of partial raw materials in the embodiment of the invention are as follows:
Yeast beta-glucan, shaanxi bran biotechnology Co., ltd., content of active substances: 99%, goods number: 03281035.
Nonylphenol polyoxyethylene ether, jinan JieWei chemical engineering Co., ltd., content of not less than 99, grade: and (5) a quality product.
Corn starch, source chemical industry Co., ltd. In Jinan sea, density: 1.25g/cm 3.
Example 1
The emamectin benzoate water dispersible granule is prepared by the following method: uniformly mixing 5kg of emamectin benzoate, 0.2kg of sorbitan monolaurate, 1.5kg of nonylphenol polyoxyethylene ether, 2kg of calcium lignosulfonate, 2kg of sodium 4-isopropylbenzene sulfonate, 0.5kg of xanthan gum and 88.8kg of filler, carrying out superfine grinding on the mixture to below 300 meshes to obtain powder by using a jet mill, adding 100kg of water, uniformly mixing, and granulating by using a disc granulator; and (3) drying the granules at 50 ℃, and screening the granules with 100 meshes by using a vibrating screen to obtain the emamectin benzoate water dispersible granule.
The filler is prepared by the following method:
s1, 2kg of yeast beta-glucan is dissolved in 100kg of water, 0.4kg of allyl glycidyl ether is added, and the mixture is stirred at room temperature at 300rpm for 1h to obtain a modified solution;
S2, dissolving 1kg of tetramethyl divinyl disilazane in 30kg of water, adding 0.5kg of potassium peroxodisulfate, introducing nitrogen at 80 ℃ at a nitrogen introducing rate of 20mL/min, and stirring for 1h at a stirring speed of 200rpm to obtain a composite solution;
S3, dropwise adding the composite solution prepared in the step S2 into the modified solution prepared in the step S1 at 80 ℃ for 10min, stirring for 6h, wherein the stirring speed is 300rpm, freeze-drying at-20 ℃ for 12h, extracting with absolute ethanol in a Soxhlet extractor for 48h, and then drying in a 70 ℃ oven for 12h to obtain the filler.
Example 2
The preparation method of the emamectin benzoate water dispersible granule is basically the same as that of the example 1, and the only difference is that: the preparation method of the filler is inconsistent.
The filler is prepared by the following method:
s1, adding 0.4kg of allyl glycidyl ether into 100kg of water, stirring at room temperature at a stirring speed of 300rpm for 1h to obtain a preparation solution;
S2, dissolving 1kg of tetramethyl divinyl disilazane in 30kg of water, adding 0.5kg of potassium peroxodisulfate, introducing nitrogen at 80 ℃ at a nitrogen introducing rate of 20mL/min, and stirring for 1h at a stirring speed of 200rpm to obtain a composite solution;
S3, dropwise adding the composite solution prepared in the step S2 into the prepared solution prepared in the step S1 at 80 ℃ for 10min, stirring for 6h, wherein the stirring speed is 300rpm, freeze-drying at-20 ℃ for 12h, extracting with absolute ethanol in a Soxhlet extractor for 48h, and then drying in a 70 ℃ oven for 12h to obtain the filler.
Example 3
The preparation method of the emamectin benzoate water dispersible granule is basically the same as that of the example 1, and the only difference is that: the preparation method of the filler is inconsistent.
The filler is prepared by the following method:
S1, 2kg of yeast beta-glucan is dissolved in 100kg of water, and stirred at room temperature at 300rpm for 1h to obtain a preparation solution;
S2, dissolving 1kg of tetramethyl divinyl disilazane in 30kg of water, adding 0.5kg of potassium peroxodisulfate, introducing nitrogen at 80 ℃ at a nitrogen introducing rate of 20mL/min, and stirring for 1h at a stirring speed of 200rpm to obtain a composite solution;
S3, dropwise adding the composite solution prepared in the step S2 into the prepared solution prepared in the step S1 at 80 ℃ for 10min, stirring for 6h, wherein the stirring speed is 300rpm, freeze-drying at-20 ℃ for 12h, extracting with absolute ethanol in a Soxhlet extractor for 48h, and then drying in a 70 ℃ oven for 12h to obtain the filler.
Example 4
The preparation method of the emamectin benzoate water dispersible granule is basically the same as that of the example 1, and the only difference is that: the preparation method of the filler is inconsistent.
The filler is prepared by the following method:
s1, 2kg of yeast beta-glucan is dissolved in 100kg of water, 0.4kg of allyl glycidyl ether is added, and the mixture is stirred at room temperature at 300rpm for 1h to obtain a modified solution;
S2, adding 0.5kg of potassium peroxodisulfate into 30kg of water, introducing nitrogen at 80 ℃ at a nitrogen rate of 20mL/min, and stirring for 1h at a stirring speed of 200rpm to obtain a solution A;
s3, dropwise adding the solution A prepared in the step S2 into the modified solution prepared in the step S1 at 80 ℃ for 10min, stirring for 6h, wherein the stirring speed is 300rpm, freeze-drying at-20 ℃ for 12h, extracting with absolute ethanol in a Soxhlet extractor for 48h, and then drying in a 70 ℃ oven for 12h to obtain the filler.
Comparative example 1
The preparation method of the emamectin benzoate water dispersible granule is basically the same as that of the example 1, and the only difference is that: the filler added in the preparation method of the water dispersible granule of emamectin benzoate is replaced by corn starch with equal amount.
Comparative example 2
The preparation method of the emamectin benzoate water dispersible granule is basically the same as that of the example 1, and the only difference is that: in the preparation method of the emamectin benzoate water dispersible granule, no filler is added, and water equivalent to the filler is adopted for replacement.
Test example 1
Field efficacy test
The results of the field efficacy tests for preventing and controlling rice stem borers using the emamectin benzoate water dispersible granules prepared in examples 1 to 4 and comparative examples 1 to 2 are shown in table 1.
The emamectin benzoate water dispersible granules prepared in examples 1-4 and comparative examples 1-2 are added with water to prepare a spraying liquid containing 6g/100kg, clear water is adopted as a blank control, a knapsack type manual sprayer is adopted to carry out uniform spraying treatment on leaf surfaces, and spraying is carried out according to 200 kg/mu of liquid medicine by taking wet leaves as the degree. The product is applied to the young larva from the hatching stage to the early stage of the young larva, and is sprayed uniformly, wet sprayed and thoroughly sprayed, and is preferably used in the evening. It is safe to most crops, but when applied, the medicine liquid should be prevented from drifting to other crops, and the medicine liquid should not be placed for too long after dilution and should be prepared at present. Rainy days or within 1 hour of prediction, do not apply the drug.
The safety interval period of the product is 7 days, and the use times of each crop period are 1. The product has moderate toxicity to birds, high toxicity to fish, high toxicity to bees and high risk to silkworms, is far away from bee sources when being applied, is forbidden in the flowering period of crops, and needs to pay close attention to the influence on nearby bees when being used. The natural enemy forbidden areas such as trichogramma are forbidden. Is applied to water bodies such as aquiculture areas, ponds and the like. The medicine application apparatus is not required to be washed in the pond, so that the pollution to water sources and the fish pond is avoided. When the product is used, protective clothing and gloves should be worn to avoid inhalation of liquid medicine. It is not edible and drinking water during administration. After the application, the hands and faces should be washed in time. Alternative uses with other pesticides with different mechanisms of action are suggested. The pregnant woman and the lactating woman are prevented from touching.
The drug effect investigation method comprises the following steps: each treatment was marked with a hanging tag, and the number of Chilo suppressalis on 6 leaves at the upper, middle and lower positions of the hanging tag was observed, ten leaves were used as one tip, and the observation was performed 7 days after the application. Meanwhile, the safety of rice in the test process, the influence on other organisms and accidents in the test process are observed and recorded.
Insect pest control effect (%) = (number of residual worms in blank control-number of residual worms in treatment group)/(number of residual worms in blank control) ×100.
The test results are shown in Table 1.
Table 1: results of field efficacy test
As can be seen from the test results in table 1, the emamectin benzoate water dispersible granule prepared in example 1 has the best field efficacy, probably because the yeast beta-glucan reacts with allyl glycidyl ether, the obtained modified compound is successfully grafted with tetramethyl divinyl disilazane to obtain a filler, pesticide molecules are encapsulated by the filler to form water dispersible granules, the pesticide molecules exist in nano filler particles in an amorphous form, and compared with the pesticide molecules, the water dispersible granules have smaller contact angle. The contact angle is reduced because the yeast beta-glucan and the tetramethyl divinyl disilazane reduce the surface energy of the water dispersible granule solution, and the spreadability of the water dispersible granule solution on the blade is increased, so that the liquid medicine is rapidly diffused and adhered on the blade. Therefore, the water dispersible granule pesticide effectively prevents the loss of the pesticide, promotes the proper dispersion of pesticide molecules and improves the pesticide efficiency.
The water dispersible granule can quickly release pesticide molecules in the early stage, and is mainly because part of pesticide molecules are not wrapped by nano particles and can be quickly released after being sprayed. The release rate of the encapsulated pesticide molecules tends to be stable, and the remaining amount of pesticide molecules is released over a longer period of time due to the biodegradability of the filler. The release mechanism is complex, and the drug release process can be practically divided into two phases: (1) burst release phase: initially the drug is released rapidly, free pesticide molecules deposit on the nanoparticle surface, resulting in rapid release of the pesticide molecules. (2) In the corrosion process under the acidic or alkaline condition, the filler is decomposed to form holes, and the corrosion solution enters into the filler molecules to cause corrosion of the inside of the filler molecules, so that pesticide molecules wrapped in the filler are released, but the release speed is slower due to the longer diffusion path. Therefore, the change of pH can change the stability of the filler, and control the release rate of pesticide molecules, thereby being suitable for the growth of different crops. The method is suitable for plants which need a large amount of pesticides at a certain stage, and can also be suitable for plants which need a small amount of pesticides in a long time.
Test example 2
Anti-ultraviolet performance test
5G of emamectin benzoate water dispersible granule prepared in the embodiment and the comparative example is added with 50g of water to prepare a solution to be detected, the solution to be detected is respectively placed at a position 20cm away from an ultraviolet lamp with the distance of 20W, after 7 hours of irradiation, 1mL of sample is taken, an ultraviolet spectrophotometer is used for measuring absorbance A of pesticide A, and the residual rate RR of the pesticide A is calculated according to a formula.
Wherein: a1 is the absorbance of the pesticide A measured after ultraviolet irradiation; a0 is the absorbance of pesticide A before irradiation.
Each sample was tested three times and averaged. The test results are shown in Table 2.
Table 2: ultraviolet resistance test results
| Test protocol | Residual Rate (%) |
| Example 1 | 78.68 |
| Example 2 | 58.36 |
| Example 3 | 69.42 |
| Example 4 | 69.01 |
| Comparative example 1 | 52.61 |
| Comparative example 2 | 52.53 |
From the test results in table 2, the residue rate of the emamectin benzoate water dispersible granule of example 1 is highest, probably because the invention a is easily decomposed by ultraviolet rays, and the pesticide molecule aqueous solution of comparative example 2 without the filler is continuously and rapidly decomposed due to no UV barrier when the ultraviolet light is continuously irradiated. In the embodiment 1, the filler is used as a shell material of pesticide molecular nano particles, and the yeast beta-glucan has good ultraviolet absorption performance, is an effective ultraviolet blocking barrier, and has a low degradation speed under UV irradiation, so that the filler has good ultraviolet shielding performance, and is a good pesticide slow-release reagent, in particular a slow-release reagent of photosensitive pesticide.
Test example 3
Encapsulation efficiency test
Adding 50g of water into 10g of emamectin benzoate water dispersible granule to prepare a solution to be detected, adding the solution to be detected into a centrifuge tube, centrifuging at a high speed of 12000r/min for 30min, measuring the concentration of supernatant after centrifugation by an ultraviolet spectrophotometer, and calculating the encapsulation efficiency lambda of the emamectin benzoate water dispersible granule according to a formula.
Wherein: lambda is the encapsulation efficiency;
M1 is the total mass of pesticide A of the solution to be detected;
m0 is the total mass of the pesticide A which is not encapsulated in the solution to be detected;
each example and comparative sample was tested three times and averaged. The test results are shown in Table 3.
Table 3: encapsulation efficiency test results
| Test protocol | Encapsulation efficiency (%) |
| Example 1 | 83.41 |
| Example 2 | 75.8 |
| Example 3 | 76.0 |
| Example 4 | 68.9 |
| Comparative example 1 | 67.1 |
| Comparative example 2 | 66.9 |
From the test results of table 3, it can be seen that the encapsulation efficiency of example 1 is the greatest, probably because the increase in the tetramethyl divinyl disilazane agent of the present invention results in an increase in the grafting ratio, resulting in higher hydrophobicity. The greater the amount of hydrophobic filler encapsulating the pesticide molecule, the greater the encapsulation efficiency of the sample, and therefore, more pesticide molecules can be encapsulated. However, the grafting ratio increases and the viscosity of the system increases, which is disadvantageous in that the reaction proceeds because the encapsulation efficiency becomes low. Therefore, in the embodiment 1 of the invention, proper material reaction and scientific proportion are selected, and the obtained encapsulation efficiency is maximum.
Claims (1)
1. The emamectin benzoate water dispersible granule is characterized by being prepared by the following method: uniformly mixing 5kg of emamectin benzoate, 0.2kg of sorbitan monolaurate, 1.5kg of nonylphenol polyoxyethylene ether, 2kg of calcium lignosulfonate, 2kg of sodium 4-isopropylbenzene sulfonate, 0.5kg of xanthan gum and 88.8kg of filler, carrying out superfine grinding on the mixture to below 300 meshes to obtain powder by using a jet mill, adding 100kg of water, uniformly mixing, and granulating by using a disc granulator; drying the particles at 50 ℃, and screening the particles with 100 meshes by using a vibrating screen to obtain emamectin benzoate water dispersible granules;
the filler is prepared by the following method:
s1, 2kg of yeast beta-glucan is dissolved in 100kg of water, 0.4kg of allyl glycidyl ether is added, and the mixture is stirred at room temperature at 300rpm for 1h to obtain a modified solution;
S2, dissolving 1kg of tetramethyl divinyl disilazane in 30kg of water, adding 0.5kg of potassium peroxodisulfate, introducing nitrogen at 80 ℃ at a nitrogen introducing rate of 20mL/min, and stirring for 1h at a stirring speed of 200rpm to obtain a composite solution;
S3, dropwise adding the composite solution prepared in the step S2 into the modified solution prepared in the step S1 at 80 ℃ for 10min, stirring for 6h, wherein the stirring speed is 300rpm, freeze-drying at-20 ℃ for 12h, extracting with absolute ethanol in a Soxhlet extractor for 48h, and then drying in a 70 ℃ oven for 12h to obtain the filler.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101361479A (en) * | 2008-09-19 | 2009-02-11 | 广州市顾地丰农药有限公司 | Water dispersion granule of methylamino avermectin benzoate and preparation method thereof |
| CN102475084A (en) * | 2010-11-25 | 2012-05-30 | 上海农乐生物制品股份有限公司 | Methylamino abamectin benzoate water dispersible granules and method for preparing same |
| CN107372542A (en) * | 2017-08-09 | 2017-11-24 | 安徽凯正农化有限公司 | 5.7% emamectin-benzoate water dispersible granules |
| CN107439568A (en) * | 2017-09-19 | 2017-12-08 | 河北兴柏农业科技有限公司 | A kind of composition pesticide containing Avermectin B2 |
| CN108684689A (en) * | 2018-07-11 | 2018-10-23 | 山东百农思达生物科技有限公司 | A kind of emamectin-benzoate water dispersible granules and preparation method thereof |
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Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101361479A (en) * | 2008-09-19 | 2009-02-11 | 广州市顾地丰农药有限公司 | Water dispersion granule of methylamino avermectin benzoate and preparation method thereof |
| CN102475084A (en) * | 2010-11-25 | 2012-05-30 | 上海农乐生物制品股份有限公司 | Methylamino abamectin benzoate water dispersible granules and method for preparing same |
| CN107372542A (en) * | 2017-08-09 | 2017-11-24 | 安徽凯正农化有限公司 | 5.7% emamectin-benzoate water dispersible granules |
| CN107439568A (en) * | 2017-09-19 | 2017-12-08 | 河北兴柏农业科技有限公司 | A kind of composition pesticide containing Avermectin B2 |
| CN108684689A (en) * | 2018-07-11 | 2018-10-23 | 山东百农思达生物科技有限公司 | A kind of emamectin-benzoate water dispersible granules and preparation method thereof |
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