CN113854297A - Nano suspending agent containing fluorine chlorantraniliprole and methoxyfenozide and preparation method thereof - Google Patents
Nano suspending agent containing fluorine chlorantraniliprole and methoxyfenozide and preparation method thereof Download PDFInfo
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- CN113854297A CN113854297A CN202111297447.6A CN202111297447A CN113854297A CN 113854297 A CN113854297 A CN 113854297A CN 202111297447 A CN202111297447 A CN 202111297447A CN 113854297 A CN113854297 A CN 113854297A
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- methoxyfenozide
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- 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
- A01N37/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids
- A01N37/36—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids
- A01N37/38—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system
- A01N37/40—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having three bonds to hetero atoms with at the most two bonds to halogen, e.g. carboxylic acids containing at least one carboxylic group or a thio analogue, or a derivative thereof, and a singly bound oxygen or sulfur atom attached to the same carbon skeleton, this oxygen or sulfur atom not being a member of a carboxylic group or of a thio analogue, or of a derivative thereof, e.g. hydroxy-carboxylic acids having at least one oxygen or sulfur atom attached to an aromatic ring system having at least one carboxylic group or a thio analogue, or a derivative thereof, and one oxygen or sulfur atom attached to the same aromatic ring system
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- 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
- A01N25/02—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 liquids as carriers, diluents or solvents
- A01N25/04—Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
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- 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
- A01N25/08—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 solids as carriers or diluents
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- 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
- A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
- A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
Abstract
The invention provides a fluorine-containing chlorantraniliprole and methoxyfenozide nano suspending agent and a preparation method thereof, belonging to the technical field of pesticide preparation. The active ingredients of the nano suspending agent comprise 1-25% of the bifendamide and 1-25% of the methoxyfenozide, 0.1-10% of the nano carrier, 0.1-20% of the solvent, 0.2-10% of the balance of the agriculturally acceptable wetting dispersant, 0.1-0.25% of the thickening agent, 0.1-0.25% of the stabilizer, 0.1-0.4% of the defoaming agent, 0.01-0.5% of the pH regulator, 0.01-0.3% of the preservative, 0.5-10% of the antifreezing agent and the balance of deionized water. The suspending agent uses nano materials to load the effective components of the pesticide, has high utilization rate and long lasting period, is convenient to use and is environment-friendly.
Description
Technical Field
A nanometer suspending agent containing fluorine chlorantraniliprole and methoxyfenozide and a preparation method thereof belong to the technical field of nanometer preparations of insecticides.
Background
The flubendiamide is a compound developed by the company of China (CN 106977)494B) Authorization has been obtained 30 days 4 months 2021. The flubendiamide belongs to benzamide insecticides, and can efficiently activate an insect ryanodine receptor so as to excessively release calcium ions in a calcium reservoir in cells, thereby causing paralysis and death of insects. The chemical name is as follows: 3-bromo-1- (3-chloropyridin-2-yl) -N- [4, 6-dichloro-3-fluoro-2- (methylcarbamoyl) phenyl]-1H-pyrazole-5-carboxamide, formula: c17H10BrCl3FN5O2Relative molecular mass (in 2009 international relative atomic mass): 521.56, melting point: 238-240 ℃ and the solubility in water is 0.711 mg/L. And the application number of the composition containing the flubendiamide and the benzoylurea insecticide is 201910056620.X on 19.1.2019, and the insecticidal composition containing the flubendiamide and the methoxyfenozide is disclosed.
Methoxyfenozide (Methoxyfenozide) is a bishydrazide insect growth regulator developed by Rohm and Haas company in America, and induces premature molting of insects to kill by simulating the function of natural molting hormone of insects and interacting with ecdysone receptor protein. Methoxyfenozide has the characteristics of strong selectivity, low toxicity, small pollution, small influence on natural enemies and beneficial organisms and the like, so that methoxyfenozide is widely applied to the control work of lepidoptera pests. Methoxyfenozide accelerates entry into the molting process leading to insect death, and also has some contact and ovicidal activity. There is no interlayer conduction or phloem systemic properties. CAS number 161050-58-4, chemical structural formula:
the suspending agent is an important preparation formulation, has good drug effect, low cost and safe production, storage and use, can be uniformly mixed and dispersed with water in any proportion, is not influenced by water quality and water temperature, is convenient to apply and is not easy to pollute the environment. The pesticide suspending agent is one of important pesticide preparations with excellent performance in water-based preparations, has rapid development, and is known as an epoch-making new formulation by being recognized in the pesticide field at home and abroad. The pesticide development of the invention is combined with the nanotechnology, and a new nano pesticide research field is formed. The appearance of the nano pesticide not only obviously reduces the dosage and improves the pesticide effect, but also gets a breakthrough in use economy, and really embodies the advantages of low use concentration, broad spectrum of killing and preventing diseases, difficult generation of drug resistance by pests and diseases, low toxicity to people and livestock, less pesticide residue, small environmental pollution and the like, thereby having important significance for researching the nano suspending agent.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide the nanoscale suspending agent containing the fluorine chlodiamide and the methoxyfenozide and the preparation method thereof. The invention innovates the dosage form of the pesticide containing the fluorine chlorantraniliprole and the methoxyfenozide, expands the high-value application of the pesticide and can meet the requirement of agricultural production.
In order to achieve the purpose of the invention, the technical scheme adopted by the invention is as follows:
the active ingredients of the nano suspending agent comprise 1-25% of the flubendiamide, 1-25% of the methoxyfenozide, 0.1-10% of a nano carrier, 0.1-20% of a solvent, and the balance of agriculturally acceptable wetting dispersant, 0.1-0.25% of a thickening agent, 0.1-0.4% of an antifoaming agent, 0.01-0.3% of a preservative, 0.5-10% of an antifreezing agent, and deionized water to complement to 100%;
further, the active ingredients of the composition are the biformamide and the methoxyfenozide, by weight, 1-25% of the biformamide, 1-25% of the methoxyfenozide, 3-5% of the nano-carrier, 1-5% of the solvent, 5-6% of the balance of the agriculturally acceptable wetting dispersant, 0.1-0.2% of the thickening agent, 0.3% of the defoaming agent, 0.01-0.05% of the preservative, 3-5% of the antifreezing agent and the balance of deionized water to 100%.
Further, the active ingredients of the pesticide composition are the biformamide and the methoxyfenozide, by weight, 1-25% of the biformamide, 1-25% of the methoxyfenozide, 3-5% of the nano carrier, 0.2% of the solvent, 5-6% of the balance of the agriculturally acceptable wetting dispersant, 0.1-0.2% of the thickening agent, 0.3% of the defoaming agent, 0.03% of the preservative, 3% of the antifreezing agent and the balance of deionized water to 100%.
Further, the weight percentage of the active ingredients in the suspending agent is 5-50%; the mass ratio of the active ingredients, namely the biformamide of the fluorine chlorine to the methoxyfenozide is 1: 30-10: 1;
further, the mass ratio of the active ingredient, namely the biformamide of the fluorine chlorine to the methoxyfenozide, is 1:30, 1:20, 1:10, 1:5, 1:3, 2:1, 3:1, 5:1 and 10: 1;
further, the mass ratio of the active ingredient, namely the biformamide of the fluorine chlorine to the methoxyfenozide is 1: 20-3: 1;
further, the mass ratio of the active ingredient, namely the biformamide of the fluorine chlorine to the methoxyfenozide is 1: 3-3: 1;
further, the nano-carrier is any one of graphene oxide, hydrophilic gas-phase nano-silica, hydrophobic gas-phase nano-silica, hydrophilic nano-titanium dioxide, lipophilic nano-titanium dioxide, nano-calcium carbonate, nano-cyclodextrin and carbon nano-tubes;
further, the solvent comprises any one of an organic solvent and vegetable oil;
further, the organic solvent is any one of toluene, acetone, dichloromethane, dimethyl sulfoxide and cyclohexanone;
further, the vegetable oil is any one of corn oil, peanut oil, cashew nut shell oil, rapeseed oil, grape seed oil, olive oil, walnut oil, zanthoxylum oil, eucalyptus oil, rosin-based vegetable oil or methylated/ethylated vegetable oil;
further, the solvent is selected from any one of peanut oil and grape seed oil;
further, the mass ratio of the solvent is 1-4%;
further, the mass ratio of the solvent is 1%, 2%, 3% and 4%;
further, the wetting dispersant comprises one or more of polyether, phenol ether phosphate, phenethyl phenol polyether phosphate, alkyl sulfonate, naphthalene sulfonate, polycarboxylate, lignosulfonate, Guerbet alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether and dioctyl sodium sulfosuccinate;
further, the polyether wetting dispersant is: pluronic PE 10500, ANTAROX P105, ANTAROX L62, Atlas G-5000, Ethylan NS-500LQ, DOWFAX D-800;
further, the isomeric tridecanol polyoxyethylene ether wetting dispersant is as follows: multsiso 13/50, multsiso 13/60, multsiso 13/70, multsiso 13/80, Lutensol TO5, Lutensol TO6, Lutensol TO7, Lutensol TO8, Lutensol TO9, Rhodasurf TDA7, Rhodasurf TDA6, Rhodasurf TDA8, Rhodasurf TDA 9;
further, the Guerbet alcohol polyoxyethylene ether wetting dispersant is: MARLOSOL DM30, MARLOSOL DM50, MARLOSOL DM70, Lutensol LXO5, Lutensol LXO6, Lutensol LXO7, Lutensol LXO8, Lutensol LXO 9;
further, the naphthalenesulfonate wetting dispersant is: amol NN 8906, Morwet D-425, 2020, Lucramul DAC 220, Dispersol BB 4;
further, the phenethyl phenol polyoxyethylene ether phosphate wetting dispersant is as follows: SopropHor SC, Emulson AG TRST, YUS-FS 3000;
further, the thickening agent comprises one or more of xanthan gum, magnesium aluminum silicate, magnesium lithium silicate, guar gum, polyvinyl alcohol, carboxymethyl cellulose and white carbon black;
further, the antifoaming agent is C10-C20Saturated fatty acid compound, silicone oil, silicone compound, C8-C10One or more of fatty alcohols;
further, the defoaming agent is an organic silicon defoaming agent;
further, the preservative is one or more of isothiazolinone, benzisothiazolinone, sodium benzoate and benzoic acid;
further, the preservative is benzisothiazolinone;
further, the antifreezing agent is one or more of alcohols, alcohol ethers, chlorinated hydrocarbons and inorganic salts;
further, the antifreezing agent is one or more of propylene glycol, ethylene glycol and urea;
a preparation method of a nanometer suspending agent containing fluorine chlorantraniliprole and methoxyfenozide comprises the following steps:
1) weighing the flubendiamide, the methoxyfenozide and the solvent according to a certain proportion, heating and stirring the mixture, completely dissolving the flubendiamide and the methoxyfenozide, adding the nano-carrier, mixing the nano-carrier and the solvent, and loading the effective components of the nano-carrier into the nano-carrier to form a mixture;
2) desolventizing the mixture obtained in the step 1 to obtain adsorption particles, coarsely crushing and mixing the adsorption particles, a wetting dispersant and deionized water, and then feeding the mixture into a sand mill to be subjected to superfine grinding and crushing until D90(90% of particles have a particle size of less than 500 nm), after grinding, pumping into a high-speed shearing machine, adding deionized water in which a thickening agent, a defoaming agent, a preservative and an anti-freezing agent are dissolved, and then carrying out high-speed shearing to obtain a suspending agent;
furthermore, the average particle diameter of the nano-carrier is 5-500 nm.
An application of a fluorine-containing chlorantraniliprole and methoxyfenozide nano suspending agent in preventing and controlling agricultural and forestry phytophagous pests; wherein said phytophagous pest larvae may be lepidopteran, coleopteran, homopteran, thysanopteran pests.
The invention relates to a nano suspending agent prepared by compounding the active ingredients of the biformamide flubendiamide and the methoxyfenozide, which is prepared by loading the pesticide active ingredients by the suspending agent through nano materials, has high utilization rate, long lasting period, convenient use and environmental protection, and can efficiently prevent and control phytophagous pests.
Compared with the prior art, the technical scheme of the invention has the following beneficial effects:
1) the dosage is obviously reduced, the use cost of the unit area of the pesticide is reduced, the investment is reduced, and the yield is improved;
2) the nano-scale suspending agent has small particle size, low surface tension, excellent permeability, wettability, leveling property and rheological property, and can directly permeate into micro pores of plants to highly disperse pesticides;
3) has the advantages of hydrolysis resistance, photolysis resistance, good stability and low loss rate;
4) the preparation method adopts a wet grinding process, optimizes the microstructure of particles in the nano suspending agent containing the flubendiamide and the methoxyfenozide, improves the suspension rate to more than 99 percent, and has obvious technical advantages.
Detailed Description
The invention provides a nano suspending agent of biformamide and methoxyfenozide, which comprises the following components in percentage by mass:
preparation example 1:
20% of biformamide methoxyfenozide nanometer suspending agent (2:3)
The formula comprises the following components: 8% of fluorochloromethrin bisamide, 12% of methoxyfenozide, 4% of hydrophilic fumed silica, 2% of peanut oil, 0.5% of polyether (ANTAROX P105), 0.5% of naphthalene sulfonate (Dispersol BB4), 3% of phenethyl phenol polyether phosphate ester salt (Soprophor SC), 2% of Guerbet alcohol polyoxyethylene ether (MARLOSOL DM70), 0.2% of xanthan gum, 3% of propylene glycol, 0.03% of benzisothiazolinone, 0.3% of an organic silicon defoamer and the balance of deionized water to 100%;
the preparation method comprises the following steps: weighing the flubendiamide, the methoxyfenozide and the solvent according to a certain proportion, heating and stirring the mixture, completely dissolving the flubendiamide and the methoxyfenozide, adding the nano-carrier, mixing the nano-carrier and the solvent, and loading the effective components of the nano-carrier into the nano-carrier to form a mixture;
desolventizing the mixture to obtain adsorbent particles, coarsely crushing and mixing the adsorbent particles, wetting dispersant and deionized water by using a homogenizer, and feeding the mixture into sandThe grinding machine is used for carrying out ultramicro grinding and crushing to D90(the grain diameter of 90 percent of particles) is less than 300nm, after grinding, pumping into a high-speed shearing machine, adding deionized water dissolved with a thickening agent, a defoaming agent, a preservative and an antifreezing agent, and then carrying out high-speed shearing to obtain the suspending agent.
Preparation example 2:
12% of cochliobolus carboximidamide methoxyfenozide nanometer suspending agent (1:5)
The formula comprises the following components: 2% of fluorochlorobinamide, 10% of methoxyfenozide, 4.2% of hydrophilic nano titanium dioxide, 2% of grape seed oil, 1% of polyether (ANTAROX P105), 2% of sodium polycarboxylate, 3% of phenethyl phenol polyether phosphate (Soprophor SC), 0.2% of xanthan gum, 3% of propylene glycol, 0.03% of benzisothiazolinone, 0.3% of organic silicon defoamer and deionized water for supplementing to 100%;
the preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 3:
20% of biformamide methoxyfenozide nanometer suspending agent (3:1)
The formula comprises the following components: 15% of fluorochloromethrin bisamide, 5% of methoxyfenozide, 4% of hydrophilic fumed silica, 2% of peanut oil, 0.5% of alkyl sodium sulfonate, 0.5% of naphthalene sulfonate (Dispersol BB4), 3% of phenethyl phenol polyether phosphate (Soprophor SC), 1.5% of Guerbet alcohol polyoxyethylene ether (Lutensol LXO5), 0.2% of polyvinyl alcohol, 3% of ethylene glycol, 0.03% of benzisothiazolinone, 0.3% of an organic silicon defoamer and the balance of deionized water to 100%;
the preparation method comprises the following steps: the same as in preparation example 1.
Preparation example 4:
20% of biformamide methoxyfenozide nanometer suspending agent (2:3)
The formula comprises the following components: 8% of fluorochloromethrin bisamide, 12% of methoxyfenozide, 4% of graphene oxide, 2% of peanut oil, 0.5% of polyether (ANTAROX P105), 0.5% of naphthalene sulfonate (Dispersol BB4), 3% of phenethyl phenol polyether phosphate ester salt (Soprophor SC), 2% of Guerbet alcohol polyoxyethylene ether (MARLOSOL DM70), 0.2% of xanthan gum, 3% of propylene glycol, 0.03% of benzisothiazolinone, 0.3% of an organic silicon defoamer and the balance of deionized water to 100%;
the preparation method comprises the following steps: the same as in preparation example 1.
Comparative example 1:
20% of biformamide methoxyfenozide suspending agent (2:3)
The formula comprises the following components: 8% of chlorofluorobisphenol, 12% of methoxyfenozide, 5% of alkylphenol polyoxyethylene, 4% of nekal BX, 0.6% of silicone oil, 1% of xanthan gum, 3% of urea and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 1.
Comparative example 2:
12% of biformamide methoxyfenozide suspending agent (1:5)
The formula comprises the following components: 2% of fluorochlordiamide, 10% of methoxyfenozide, 5% of lignosulfonate, BX 3% of nekal, 0.5% of silicone oil, 1.2% of xanthan gum, 3% of ethylene glycol and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 1.
Comparative example 3:
40% Flucloxacarbdiamide methoxyfenozide suspending agent (3:1)
The formula comprises the following components: 30% of flubendiamide, 10% of methoxyfenozide, 4% of alkylphenol polyoxyethylene, 2.8% of sodium dodecyl sulfate, 0.7% of silicone oil, 1% of xanthan gum, 4% of urea and the balance of deionized water.
The preparation method comprises the following steps: the same as in preparation example 1.
Quality testing test
1) And (3) appearance test determination:
the test is carried out according to NY/T1860.3-2016, guide rule for determination of physicochemical properties of pesticides, part 3: appearance (appearance)
And (3) color determination: a certain test substance is put in a 100mL beaker and placed on a white background, and the color of the test substance is evaluated by comparing according to a standard color comparison card.
And (3) physical state determination: a certain amount of the test substance was put in a 100mL beaker, and the physical state of the test substance was evaluated.
And (3) odor determination: a certain amount of the test substance is put in a 100mL beaker and placed in front of the nose, and the mouth of the beaker is lightly fanned by the right hand to evaluate the smell of the test substance.
2) And (3) suspension rate determination:
the test is based on GB/T14825-2006 method for determining the suspension rate of pesticide
Accurately weighing 1.0g (accurate 0.0002g) of the test object, placing the test object in a measuring cylinder filled with 100mL of 30 +/-2 ℃ standard hard water, diluting the test object to a scale with the 30 +/-2 ℃ standard hard water, covering a plug, and turning the measuring cylinder upside down for 30 times within 1min by taking the middle part of the measuring cylinder as an axis. And opening the plug, vertically placing into a constant temperature water bath without vibration, preventing direct irradiation of sunlight, and standing for 30 min. The 9/10 (i.e., 225mL) suspension of the contents was removed with a pipette within 10-15 s without shaking or lifting the contents of the cylinder to ensure that the top of the pipette was always a few millimeters below the liquid surface. The remaining 1/10 (i.e., 25mL) suspension and precipitate were transferred, all poured into a clean 100mL volumetric flask, dissolved in methanol and diluted to the mark, shaken well and filtered.
According to GB/T19137-. And 7d, taking out the centrifugal tube, recovering to room temperature, and testing the physicochemical index of the suspension rate.
According to GB/T19136-2003 'method for measuring stability of pesticide thermal storage', a glass dish serum bottle is placed in a biochemical incubator at the temperature of (54 +/-2) ° C for 14 days, taken out, wiped and weighed, and a test object with unchanged quality is tested within 24 hours to finish the test of specified items such as the content of active ingredients.
TABLE 1 measurement results of appearance test
TABLE 2 determination of the suspension percentage of the suspending agent
| Serial number | Name (R) | The suspension rate% | Stability to Heat/Cold storage | Particle size |
| Preparation example 1 | 20% of biformamide methoxyfenozide nanometer suspending agent (2:3) | 99.86 | Qualified | D90＜300nm |
| Preparation example 2 | 12% of cochliobolus carboximidamide methoxyfenozide nanometer suspending agent (1:5) | 99.23 | Qualified | D90＜300nm |
| Preparation example 3 | 20% of biformamide methoxyfenozide nanometer suspending agent (3:1) | 99.46 | Qualified | D90＜300nm |
| Preparation example 4 | 20% of biformamide methoxyfenozide nanometer suspending agent (2:3) | 99.57 | Qualified | D90＜300nm |
| Comparative example 1 | 20% of biformamide methoxyfenozide suspending agent (2:3) | 87.56 | Qualified | D90＜5μm |
| Comparative example 2 | 12% of biformamide methoxyfenozide suspending agent (1:5) | 84.33 | Qualified | D90＜5μm |
| Comparative example 3 | 40% Flucloxacarbdiamide methoxyfenozide suspending agent (3:1) | 83.56 | Qualified | D90＜5μm |
Indoor Activity test 1
The test insect age is as follows: breeding sensitive population of Pieris rapae in room for several generations, namely Pieris rapae second-instar larva (cabbage caterpillar);
soaking fresh cauliflower leaves in the liquid medicine for 10s by using tweezers, taking out, naturally airing the liquid medicine, placing the cauliflower leaves in a culture dish padded with moisture-preserving filter paper, placing 20 cabbage caterpillars in the liquid medicine for 5s, absorbing the redundant liquid medicine by using the filter paper, and placing the test insects in the culture dish soaked with leaves at a corresponding concentration; each treatment was repeated 4 times, with a blank treatment as a control.
The treated test insects are placed in an artificial intelligent culture room with the temperature of 26 +/-1 ℃, the illumination time L: D: 16h:8h and the relative humidity of 60 percent for feeding.
Investigating the death condition of the test insects 48 hours after the treatment of the medicament, judging the death standard of the test insects to be that the insects shrink obviously or the needles can not climb normally, and recording the number of the dead insects.
Data statistics and analysis: the blank control mortality rate is less than 5% without correction; the blank control mortality rate is 5% -20%, and the mortality rate needs to be corrected; the blank mortality rate was above 20%, and the test was repeated.
The calculation formula is as follows:
by LC50The relatively small-value agent is a standard agent, and the virulence index TI thereof is 100.
Theoretical virulence index TTI ═ TI for the mixturesA×PA+TIB×PB
In the formula: pA、PBRespectively the weight ratio of the active ingredient A, B in the composition.
Table 3 indoor toxicity test results of the compounded compound of the biformamide of the fluorine chlorine worm and the methoxyfenozide to the cabbage caterpillar
Table 3 shows that the biformamide and the methoxyfenozide have higher insecticidal activity on cabbage caterpillars, synergistic effect is shown when the mixture ratio is 1: 30-10: 1, and when the mixture ratio is 1: 3-3: 1, the cotoxicity coefficients are all larger than 150, which indicates that the biformamide and the methoxyfenozide show obvious synergistic effect in the mixture ratio range.
Field example 1
Prevention and control of cauliflower cabbage caterpillar by field test
Test subjects: cabbage worm;
the experiment is carried out in a high willow-Zhendong kalimeris village cauliflower planting base in the Weifang city in Shandong province, the fertility of the experimental field is medium, and the cultivation conditions are consistent.
The test is totally provided with 4 mixing treatments, 3 comparison treatments, 4 times of repetition and random arrangement, and the area of a cell is 20m2. The experiment is that the pesticide is applied for 1 time at the early generation stage of the cabbage caterpillar, and the water consumption is 675kg/hm2。
The pesticide application apparatus is a WS-16D guard electric sprayer, the spray head is a single fan-shaped fog spray head, the working pressure is 0.15-0.4Mpa, and the dosage is accurately measured according to the dosage requirement of the pesticide and the area of a cell.
When dispensing, firstly adding clean water with one third of actual water consumption into the sprayer, adding a little water into the small measuring cup to uniformly stir the medicament, pouring the medicament into the sprayer, and finally adding the rest water and uniformly mixing.
When the pesticide is applied, the control is sprayed firstly, and the spraying is carried out from low concentration to high concentration in sequence, and the constant spraying method is adopted, and the uniform spraying is carried out at a constant speed according to the calculated step speed. When different medicaments are replaced, the sprayer is cleaned for three times, and water in the spray rod is completely sprayed out.
The weather was good during the test, and the daily average temperature was 24 ℃ on the day of application.
The investigation method comprises the following steps: the population base number is investigated before the pesticide application, five surveys are carried out in each cell, 2 cauliflowers are investigated in each spot, and the number of live insects is investigated at 5d and 20d after the pesticide application.
The drug effect calculation method comprises the following steps:
during the test period, the growth of the cauliflower in each treatment cell is observed to be good, and no phytotoxicity is generated in each treatment.
TABLE 4 field test results for cabbage worm control with different treatments
The field test results of different treatments for controlling cabbage caterpillars in Table 4 show that the suspending agent compounded by the fluorochlorobinamide and the methoxyfenozide can effectively control the cabbage caterpillars, wherein the control effect of the nano suspending agent is better than that of the suspending agent, and the control effects of the preparation examples 1-4 are all more than 87% after 5 days of application, so that the suspending agent shows better quick action; the control effect of the nano suspending agents of the preparation examples 1 to 4 is 100 percent along with the increase of time 20 days after the application. The nano suspending agent of the bifloram and the methoxyfenozide has better quick-acting property and lasting property on the cabbage caterpillar. And has no adverse effect on target crops in the application range of the test.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.
Claims (10)
1. The nanometer suspending agent containing the flubendiamide and the methoxyfenozide is characterized in that active ingredients of the nanometer suspending agent are the flubendiamide and the methoxyfenozide, and the weight percentage of the active ingredients are 1-25% of the flubendiamide, 1-25% of the methoxyfenozide, 0.1-10% of a nanometer carrier, 0.1-20% of a solvent, 0.2-10% of a wetting dispersant acceptable in agriculture, 0.1-0.25% of a thickening agent, 0.1-0.4% of an antifoaming agent, 0.01-0.3% of a preservative, 0.5-10% of an antifreezing agent, and the balance of deionized water is added to 100%.
2. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the weight percentage of the active ingredients in the suspending agent is 5-50%; the mass ratio of the active ingredients, namely the biformamide of the fluorine chlorine to the methoxyfenozide is 1: 30-10: 1;
preferably, the mass ratio of the active ingredient, namely the biformamide of the fluorine chlorine to the methoxyfenozide is 1: 3-3: 1.
3. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the nano-carrier is any one of graphene oxide, hydrophilic gas-phase nano-silica, hydrophobic gas-phase nano-silica, hydrophilic nano-titanium dioxide, lipophilic nano-titanium dioxide, nano-calcium carbonate, nano-cyclodextrin and carbon nano-tubes.
4. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the solvent comprises any one of organic solvent and vegetable oil or a mixture thereof;
the organic solvent is any one of toluene, acetone, dichloromethane, dimethyl sulfoxide and cyclohexanone;
the vegetable oil is any one of corn oil, peanut oil, cashew nut shell oil, rapeseed oil, grape seed oil, olive oil, walnut oil, zanthoxylum oil, eucalyptus oil, rosin-based vegetable oil or methylated/ethylated vegetable oil.
5. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the wetting dispersant comprises one or more of polyether, phenol ether phosphate, phenethyl phenol polyether phosphate, alkyl sulfonate, naphthalene sulfonate, polycarboxylate, lignosulfonate, Guerbet alcohol polyoxyethylene ether, isomeric alcohol polyoxyethylene ether and dioctyl sodium sulfosuccinate.
6. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the thickening agent comprises any one of xanthan gum and polyvinyl alcohol.
7. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the defoaming agent is an organic silicon defoaming agent.
8. The fluorine-containing clofenac diamide and methoxyfenozide nano suspending agent as claimed in claim 1, is characterized in that: the preservative is benzisothiazolinone; the antifreezing agent is any one of propylene glycol and ethylene glycol.
9. The preparation method of the nano suspending agent containing the fluorine clofenac bisamide and the methoxyfenozide, which is characterized by comprising the following steps:
1) weighing the flubendiamide, the methoxyfenozide and the solvent according to a certain proportion, heating and stirring to dissolve the flubendiamide and the methoxyfenozide, adding the nano-carrier, mixing, and loading the effective components in the nano-carrier to form a mixture;
2) desolventizing the mixture obtained in the step 1 to obtain adsorption particles, coarsely crushing and mixing the adsorption particles, a wetting dispersant and deionized water, and then feeding the mixture into a sand mill to be subjected to superfine grinding and crushing until D90(90% of the particles have a size of less than 500 nm) and after grinding is complete, the mixture is pumped upAnd adding deionized water in which a thickening agent, a defoaming agent, a preservative and an antifreezing agent are dissolved into a quick shearing machine, and then carrying out high-speed shearing to prepare the suspending agent.
10. The Nanosuspension agent containing the chlorofluorobisphenol and methoxyfenozide of claim 1, wherein the average particle size of the nanocarrier is 5-500 nm.
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| CN114431248A (en) * | 2022-02-07 | 2022-05-06 | 陕西先农生物科技有限公司 | Suspending agent containing abamectin and chlorantraniliprole |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN114431248A (en) * | 2022-02-07 | 2022-05-06 | 陕西先农生物科技有限公司 | Suspending agent containing abamectin and chlorantraniliprole |
| CN114431248B (en) * | 2022-02-07 | 2023-09-01 | 陕西先农生物科技有限公司 | Suspending agent containing avermectin and chlorantraniliprole |
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