CN116548450A - Preparation method and application of nano suspending agent - Google Patents
Preparation method and application of nano suspending agent Download PDFInfo
- Publication number
- CN116548450A CN116548450A CN202211223367.0A CN202211223367A CN116548450A CN 116548450 A CN116548450 A CN 116548450A CN 202211223367 A CN202211223367 A CN 202211223367A CN 116548450 A CN116548450 A CN 116548450A
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- China
- Prior art keywords
- chlorantraniliprole
- agent
- tolfenpyrad
- suspending agent
- test
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- 239000000375 suspending agent Substances 0.000 title claims abstract description 88
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000005886 Chlorantraniliprole Substances 0.000 claims abstract description 67
- PSOVNZZNOMJUBI-UHFFFAOYSA-N chlorantraniliprole Chemical compound CNC(=O)C1=CC(Cl)=CC(C)=C1NC(=O)C1=CC(Br)=NN1C1=NC=CC=C1Cl PSOVNZZNOMJUBI-UHFFFAOYSA-N 0.000 claims abstract description 67
- 241000500437 Plutella xylostella Species 0.000 claims abstract description 52
- WPALTCMYPARVNV-UHFFFAOYSA-N tolfenpyrad Chemical compound CCC1=NN(C)C(C(=O)NCC=2C=CC(OC=3C=CC(C)=CC=3)=CC=2)=C1Cl WPALTCMYPARVNV-UHFFFAOYSA-N 0.000 claims abstract description 51
- 240000007124 Brassica oleracea Species 0.000 claims abstract description 37
- 235000003899 Brassica oleracea var acephala Nutrition 0.000 claims abstract description 37
- 235000011301 Brassica oleracea var capitata Nutrition 0.000 claims abstract description 37
- 235000001169 Brassica oleracea var oleracea Nutrition 0.000 claims abstract description 37
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 239000004576 sand Substances 0.000 claims abstract description 12
- 230000001276 controlling effect Effects 0.000 claims abstract description 11
- 239000002002 slurry Substances 0.000 claims abstract description 9
- 239000002518 antifoaming agent Substances 0.000 claims abstract description 7
- 239000002562 thickening agent Substances 0.000 claims abstract description 7
- 239000006185 dispersion Substances 0.000 claims abstract description 6
- 238000003801 milling Methods 0.000 claims abstract description 6
- 238000001514 detection method Methods 0.000 claims abstract description 4
- 239000002270 dispersing agent Substances 0.000 claims abstract description 4
- 239000002994 raw material Substances 0.000 claims abstract description 4
- 238000003756 stirring Methods 0.000 claims abstract description 4
- 239000000080 wetting agent Substances 0.000 claims abstract description 4
- 239000012752 auxiliary agent Substances 0.000 claims abstract description 3
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- 238000002474 experimental method Methods 0.000 description 6
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- ABUGVBRDFWGJRD-CHOYNLESSA-N [9-[(2r,3r,4s,5r)-3,4-dihydroxy-5-methyloxolan-2-yl]-2-(2,4-dinitrophenyl)sulfanylpurin-6-yl] [hydroxy(phosphonooxy)phosphoryl] hydrogen phosphate Chemical compound O[C@@H]1[C@H](O)[C@@H](C)O[C@H]1N1C2=NC(SC=3C(=CC(=CC=3)[N+]([O-])=O)[N+]([O-])=O)=NC(OP(O)(=O)OP(O)(=O)OP(O)(O)=O)=C2N=C1 ABUGVBRDFWGJRD-CHOYNLESSA-N 0.000 description 3
- 238000013461 design Methods 0.000 description 3
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- 239000007788 liquid Substances 0.000 description 3
- 238000005259 measurement Methods 0.000 description 3
- 238000010561 standard procedure Methods 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 2
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- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- 241000361919 Metaphire sieboldi Species 0.000 description 2
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- 241000700159 Rattus Species 0.000 description 2
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 230000005791 algae growth Effects 0.000 description 2
- 238000004364 calculation method Methods 0.000 description 2
- 235000013339 cereals Nutrition 0.000 description 2
- 239000013530 defoamer Substances 0.000 description 2
- 238000007865 diluting Methods 0.000 description 2
- 238000001647 drug administration Methods 0.000 description 2
- 235000013305 food Nutrition 0.000 description 2
- 229930182470 glycoside Natural products 0.000 description 2
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- 235000013311 vegetables Nutrition 0.000 description 2
- 239000000230 xanthan gum Substances 0.000 description 2
- 229920001285 xanthan gum Polymers 0.000 description 2
- 229940082509 xanthan gum Drugs 0.000 description 2
- 235000010493 xanthan gum Nutrition 0.000 description 2
- IWOUTIHKEQOMCY-UHFFFAOYSA-N 2-ethyl-3,4,5-triphenylphenol Chemical compound C1(=CC=CC=C1)C=1C(=C(C(=C(C1)O)CC)C1=CC=CC=C1)C1=CC=CC=C1 IWOUTIHKEQOMCY-UHFFFAOYSA-N 0.000 description 1
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- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 241000256259 Noctuidae Species 0.000 description 1
- IGFHQQFPSIBGKE-UHFFFAOYSA-N Nonylphenol Natural products CCCCCCCCCC1=CC=C(O)C=C1 IGFHQQFPSIBGKE-UHFFFAOYSA-N 0.000 description 1
- 241000283973 Oryctolagus cuniculus Species 0.000 description 1
- 229910019142 PO4 Inorganic materials 0.000 description 1
- 231100000674 Phytotoxicity Toxicity 0.000 description 1
- 241000255969 Pieris brassicae Species 0.000 description 1
- 229920003171 Poly (ethylene oxide) Polymers 0.000 description 1
- 206010070834 Sensitisation Diseases 0.000 description 1
- 206010040880 Skin irritation Diseases 0.000 description 1
- 206010070835 Skin sensitisation Diseases 0.000 description 1
- DBMJMQXJHONAFJ-UHFFFAOYSA-M Sodium laurylsulphate Chemical compound [Na+].CCCCCCCCCCCCOS([O-])(=O)=O DBMJMQXJHONAFJ-UHFFFAOYSA-M 0.000 description 1
- 229920000142 Sodium polycarboxylate Polymers 0.000 description 1
- 241000209140 Triticum Species 0.000 description 1
- 235000021307 Triticum Nutrition 0.000 description 1
- 230000000895 acaricidal effect Effects 0.000 description 1
- 239000000642 acaricide Substances 0.000 description 1
- 229960000583 acetic acid Drugs 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 239000000654 additive Substances 0.000 description 1
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- 239000006229 carbon black Substances 0.000 description 1
- 239000004359 castor oil Substances 0.000 description 1
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- 239000003337 fertilizer Substances 0.000 description 1
- NVVZQXQBYZPMLJ-UHFFFAOYSA-N formaldehyde;naphthalene-1-sulfonic acid Chemical compound O=C.C1=CC=C2C(S(=O)(=O)O)=CC=CC2=C1 NVVZQXQBYZPMLJ-UHFFFAOYSA-N 0.000 description 1
- 239000012362 glacial acetic acid Substances 0.000 description 1
- ZEMPKEQAKRGZGQ-XOQCFJPHSA-N glycerol triricinoleate Natural products CCCCCC[C@@H](O)CC=CCCCCCCCC(=O)OC[C@@H](COC(=O)CCCCCCCC=CC[C@@H](O)CCCCCC)OC(=O)CCCCCCCC=CC[C@H](O)CCCCCC ZEMPKEQAKRGZGQ-XOQCFJPHSA-N 0.000 description 1
- 230000012010 growth Effects 0.000 description 1
- WGCNASOHLSPBMP-UHFFFAOYSA-N hydroxyacetaldehyde Natural products OCC=O WGCNASOHLSPBMP-UHFFFAOYSA-N 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 230000007653 larval development Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 230000003020 moisturizing effect Effects 0.000 description 1
- 231100000286 mucous membrane, eye irritation or corrosion testing Toxicity 0.000 description 1
- 231100000989 no adverse effect Toxicity 0.000 description 1
- SNQQPOLDUKLAAF-UHFFFAOYSA-N nonylphenol Chemical compound CCCCCCCCCC1=CC=CC=C1O SNQQPOLDUKLAAF-UHFFFAOYSA-N 0.000 description 1
- 230000017448 oviposition Effects 0.000 description 1
- 239000008194 pharmaceutical composition Substances 0.000 description 1
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 1
- 239000010452 phosphate Substances 0.000 description 1
- 230000008635 plant growth Effects 0.000 description 1
- 229920005646 polycarboxylate Polymers 0.000 description 1
- 229920002503 polyoxyethylene-polyoxypropylene Polymers 0.000 description 1
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- 230000001850 reproductive effect Effects 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
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- 231100000475 skin irritation Toxicity 0.000 description 1
- 231100000370 skin sensitisation Toxicity 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
- 235000010234 sodium benzoate Nutrition 0.000 description 1
- 159000000000 sodium salts Chemical class 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000007619 statistical method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- BDHFUVZGWQCTTF-UHFFFAOYSA-M sulfonate Chemical compound [O-]S(=O)=O BDHFUVZGWQCTTF-UHFFFAOYSA-M 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
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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
- A01N43/48—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
-
- 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
-
- 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
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/30—Against vector-borne diseases, e.g. mosquito-borne, fly-borne, tick-borne or waterborne diseases whose impact is exacerbated by climate change
Landscapes
- Life Sciences & Earth Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Health & Medical Sciences (AREA)
- Engineering & Computer Science (AREA)
- Zoology (AREA)
- General Health & Medical Sciences (AREA)
- Environmental Sciences (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Chemical & Material Sciences (AREA)
- Dispersion Chemistry (AREA)
- Toxicology (AREA)
- Insects & Arthropods (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention relates to the technical field of pesticides, and discloses a preparation method and application of a nano suspending agent. The nanometer suspending agent comprises chlorantraniliprole, tolfenpyrad, dispersing agent, wetting agent, defoaming agent, thickening agent and water, and can be added with antifreezing agent and preservative; wherein the weight ratio of chlorantraniliprole to tolfenpyrad is 1:1-1:3. The preparation method of the nanometer suspending agent comprises the following steps: firstly, putting water, an auxiliary agent, chlorantraniliprole and tolfenpyrad raw material into a stirring tank for high-speed shearing, and forming primary dispersion after full dispersion; then the slurry is conveyed into a sand mill by a diaphragm pump to be crushed, the sand milling feeding speed is regulated to ensure that the sand milling fineness is controlled to be 0.1-1 mu m, the slurry is finely ground by a rod pin type sand mill, the grain diameter is controlled to be 100-500 nanometers, and the grain size is confirmed to meet the requirement; and finally, conveying the slurry to a preparation kettle, adding a thickening agent and a defoaming agent, adjusting the viscosity of the materials, sampling, and performing quality detection to obtain a finished product. The nanometer suspending agent is used for preventing and controlling cabbage plutella xylostella, has small particle size, strong adhesive force and good dispersibility, can effectively control pests, improves the effect of preventing and controlling cabbage plutella xylostella, is safe to crops and natural enemies, has long lasting period and small residue.
Description
Technical Field
The invention belongs to the technical field of pesticides, and particularly relates to a preparation method and application of a nano suspending agent.
Background
The chlorantraniliprole is high-efficiency broad-spectrum, has good control effect on noctuidae, borer moth, fruit moth, leaf moth, pink moth, plutellaceae, wheat moth, lepidoptera weevilidae and the like, and can also control coleoptera weevilidae and leaf beetle; the family of the Lepidoptera, the family of the Lepidoptera; various non-lepidopteran pests such as bemisia tabaci.
The tolfenpyrad is a novel pyrazole heterocyclic insecticidal acaricide, has a contact insecticidal effect, has a good effect on lepidoptera pests and the like, has a long lasting period, and can inhibit the pests from feeding.
Cabbage plutella xylostella is commonly generated throughout the country, and the generation of 4-19 years is different. 4-5 generations occur in north, 9-14 generations in Yangtze river basin, 17 generations in south China and 18-19 generations in taiwan. Overwintering in the northern part by using pupae in fallen leaves of residual plants and weed clusters; the insect states can be seen throughout the year in the south, and the phenomenon of overwintering is avoided. The full period of injury in the whole year is different from region to region, the regions in northeast and North China are serious for 5-6 months and 8-9 months, and the spring is heavier than the autumn. The larvae, pupae and adults can live through winter and summer without diapause. The occurrence of the injury in the whole year clearly shows two peaks, the first time is from 5 middle ten days to 6 late ten days; the second time from the last ten days of 8 months to the last ten days of 10 months (positive cruciferous vegetable large-area cultivation season). The autumn injury is more serious than the spring injury in the general year. The development temperature of the plutella xylostella is 20-30 ℃, and the plutella xylostella completes 1 generation for about 20d in two full-growing periods.
In the prior art, the main factors that the plutella xylostella is difficult to control are as follows:
1) The body is small, and only a small amount of food can survive, so that enemy is easy to avoid;
2) The life cycle is short, when the temperature of eating the cabbage is 28-30 ℃, the first generation is finished for only 10 days at the highest speed;
3) The reproductive capacity is strong, the average spawning quantity per female is 220, and the spawning quantity per female is distributed;
4) The oviposition period of the overwintering adults can reach 90 days, so that serious generation overlap is caused, and the prevention and the control are difficult;
5) The ecological adaptability is strong, the cold of minus 15 ℃ can be stiff in winter, and the food can be taken in the environment of minus 1.4 ℃;
6) The pesticide has strong drug resistance, the natural enemies are killed greatly due to the long-term prevention and control by using chemical pesticides, the plutella xylostella is harmful for the day and even for a day, and very high level resistance is generated on various chemical pesticides quickly, and the plutella xylostella gradually replaces cabbage caterpillar to become vegetable No. 1 pests due to large occurrence area, long harmful time and difficult prevention and control.
The applicant finds that by continuously and innovatively researching and mixing chlorantraniliprole and tolfenpyrad with completely different action mechanisms, the product has small particle size, strong adhesive force and good dispersibility, can effectively control pests, improves the effect of preventing and controlling cabbage plutella xylostella, is safe to crops and natural enemies, has long lasting period and small residue, reduces pollution of medicaments to the environment, and is safe to the natural enemies.
Disclosure of Invention
The invention aims to provide a preparation method and application of a nano suspending agent, which can effectively prevent cabbage plutella xylostella, has small particle size, strong adhesive force and good dispersibility, can effectively control pests, improves the effect of preventing and controlling cabbage plutella xylostella, is safe to crops and natural enemies, has long lasting period and small residue.
The technical scheme of the invention is as follows:
a preparation method and application of a nanometer suspending agent are characterized in that: the nanometer suspending agent comprises chlorantraniliprole, tolfenpyrad, dispersing agent, wetting agent, defoaming agent, thickening agent and water, and can be added with antifreezing agent and preservative; wherein the weight ratio of chlorantraniliprole to tolfenpyrad is 1:1-1:3, and the preferable ratio is 2:3.
Further, the total content of chlorantraniliprole and tolfenpyrad in the nano suspending agent is 10% -50%, and the preferable total content is 25%.
Further, the preparation method of the nanometer suspending agent comprises the following steps: firstly, putting water, an auxiliary agent, chlorantraniliprole and tolfenpyrad raw material into a stirring tank for high-speed shearing, and forming primary dispersion after full dispersion; then the slurry is conveyed into a sand mill by a diaphragm pump to be crushed, the sand milling feeding speed is regulated to ensure that the sand milling fineness is controlled to be 0.1-1 mu m, the slurry is finely ground by a rod pin type sand mill, the grain diameter is controlled to be 100-500 nanometers, and the grain size is confirmed to meet the requirement; and finally, conveying the slurry to a preparation kettle, adding a thickening agent and a defoaming agent, adjusting the viscosity of the materials, sampling, and performing quality detection to obtain a finished product.
Further, the nanometer suspending agent is used for preventing and controlling cabbage plutella xylostella.
Further, the dosage of the active ingredients of the nanometer suspending agent is 37.5-75 g/hectare.
Further, the water consumption of the nano suspending agent for preventing and controlling cabbage diamondback moth is 675-900 liters per hectare, and the water consumption is preferably 750-900 liters per hectare.
The nanometer suspending agent comprises the following components in percentage by weight: 2.5 to 25 percent of chlorantraniliprole, 5 to 37.5 percent of tolfenpyrad, 1 to 10 percent of dispersing agent, 1 to 10 percent of wetting agent, 0.1 to 2 percent of defoaming agent, 0.2 to 3 percent of thickening agent, 0 to 10 percent of antifreezing agent, 0 to 2 percent of preservative, 0 to 2 percent of PH regulator and the balance of water.
Compared with the prior art, the composition provided by the invention has the following beneficial effects: (1) Compared with a single dose, the composition has obvious synergism on cabbage plutella xylostella, and the control effect is obviously improved; (2) The pesticide is low in toxicity and high in efficiency, the pesticide dosage is reduced, the residual quantity of the pesticide on crops is reduced, and the safety interval period is short; (3) has quick and long-acting effects; (4) safe to natural enemies; and (5) the product has small particle size, good dispersibility and strong adhesive force.
Detailed Description
The present invention will be further illustrated with reference to examples, but the present invention is not limited thereto.
Application example one
EXAMPLE 1 25% Chlorantraniliprole/tolfenpyrad suspension
95% chlorantraniliprole is folded by 10%, 98% tolfenpyrad is folded by 15%, polycarboxylate 3%, castor oil polyoxyethylene ether 2%, ethylene glycol 4%, polyvinyl alcohol 0.4%, magnesium aluminum silicate 0.4%, sodium benzoate 0.2%, citric acid 0.2%, organic silicone defoamer 0.3% and water balance are added, and the 25% chlorantraniliprole-tolfenpyrad suspending agent is prepared.
EXAMPLE 2 25% Chlorantraniliprole/tolfenpyrad suspension
95% chlorantraniliprole is folded by 10%, 98% tolfenpyrad is folded by 15%, alkyl naphthalene sulfonate formaldehyde polymer is 2.5%, polyarylphenol polyoxyethylene ether is 2%, propylene glycol is 5%, xanthan gum is 0.2%, magnesium aluminum silicate is 0.6%, C10-20 saturated fatty acid compound is 0.3%, and the balance is water, so that 25% chlorantraniliprole-tolfenpyrad suspending agent is prepared.
EXAMPLE 3 10% Chlorantraniliprole-tolfenpyrad suspension
95% chlorantraniliprole is folded by 5%, 98% tolfenpyrad is folded by 5%, nonylphenol polyoxyethylene ether phosphate is 1.5%, sodium dodecyl sulfate is 3%, urea is 5%, white carbon black is 1%, glacial acetic acid is 0.5%, C8-10 fatty alcohols are 0.3% and the balance is water, so that the 10% chlorantraniliprole-tolfenpyrad suspending agent is prepared.
EXAMPLE 4 40% Chlorantraniliprole/tolfenpyrad suspension
95% chlorantraniliprole is folded by 10%, 98% tolfenpyrad is folded by 30%, sodium polycarboxylate is 1.5%, naphthalene sulfonic acid formaldehyde condensate sodium salt segmented copolymer is 2%, alkyl glycoside is 2%, fatty alcohol polyoxyethylene ether sodium sulfonate is 1%, glycerol is 3%, xanthan gum is 0.2%, magnesium aluminum silicate is 0.3%, silicone defoamer is 0.2%, and the balance is water, so that 25% chlorantraniliprole-tolfenpyrad suspending agent is prepared.
EXAMPLE 5 50% Chlorantraniliprole/tolfenpyrad suspension
The 50% chlorantraniliprole suspending agent is prepared from the raw materials of 95% chlorantraniliprole of 20%, 98% tolfenpyrad of 30%, alkyl naphthalene sulfonate of 2%, polyoxyethylene polyoxypropylene ether block copolymer of 1%, triphenyl ethylphenol polyoxypropylene polyoxyethylene block polymer of 1.5%, alkyl glycoside of 2%, glycol of 5%, polyvinyl alcohol of 0.1%, magnesium aluminum silicate of 0.5%, C8-10 fatty alcohols of 0.3%, citric acid of 0.1% and the balance of water.
Implementation example II:
indoor combined toxicity determination experiment for chlorantraniliprole, tolfenpyrad and mixed cabbage plutella xylostella
1 purpose of test
The toxicity of chlorantraniliprole and tolfenpyrad and different mixed combinations thereof to plutella xylostella is measured indoors, the synergism is evaluated, the suitability of the chlorantraniliprole and tolfenpyrad is clear, and scientific basis is provided for the research and development of chlorantraniliprole and tolfenpyrad mixture.
2 experimental conditions
2.1 test targets
The larvae of plutella xylostella (Plutella xylostella) are collected in the field, cabbage is used for breeding a multi-generation strain indoors, and 3-year larvae are taken for a biological test.
2. Culture conditions
The culture conditions of the tested target and the tested target are that the temperature is 25+/-1 ℃, the relative humidity is 60% -80%, and the illumination period is L:D= (16:8) h.
3 test design
3.1 test Agents
Chlorantraniliprole (Chlorantraniliprole) 95.3% technical and tolfenpyrad (tolfenpyrad) 98% technical.
3.2 pharmaceutical formulation
0.0105g of chlorantraniliprole 95.3% is weighed, dissolved in 0.5mL of DMF, added with 0.2mL of Tween80 emulsifier, evenly stirred, added with 99.3mL of clear water to prepare 100mg/L of mother liquor, then 4mL of mother liquor is added into 96mL of water containing 0.1% Tween80 emulsifier to prepare 4mg/L of test solution, and the test solution is diluted into 2, 1, 0.5, 0.25 and 0.125mg/L of water containing 0.1% Tween80 emulsifier according to a proportion of 2 times, so that 6 concentrations are tested.
Weighing 0.0204g of tolfenpyrad 98% raw medicine, dissolving with 0.5mLDMF, adding 0.2 mLTweeen 80 emulsifier, stirring uniformly, adding 199.3mL of clear water to prepare 100mg/L mother liquor, adding 20mL of water containing 0.1% Tween80 emulsifier into 80mg/L mother liquor to prepare 80mg/L test solution, and diluting the test solution with water containing 0.1% Tween80 emulsifier according to a proportion of 2 times to prepare 40, 20, 10, 5 and 2.5mg/L solutions, wherein 6 concentrations are tested;
according to the ratio of 3:2, 1:1, 2:3, 1:2 and 1:3 of chlorantraniliprole to 2mL of chlorantraniliprole mother liquor, respectively measuring 4.8, 4, 3.2, 2.67 and 2mL of chlorantraniliprole mother liquor, respectively measuring 3.2, 4.8, 5.33 and 6mL of chlorantraniliprole mother liquor, mixing the two mother liquors, supplementing water with emulsifying agent to 100mL, preparing 8mg/L of test solution, respectively diluting the test solution with water containing 0.1% Tween80 emulsifying agent according to the ratio of 2 times to 4, 2, 1, 0.5 and 0.25mg/L, and carrying out test.
99.5mL of water containing 0.1% Tween80 emulsifier was added to a beaker containing 0.5mL of DMF as a blank.
4 test method
With reference to "evaluation of pesticide biological Activity SOP" and NY/T1154.14-2008, dip She Diefa is used. The cabbage leaves are beaten into leaf discs by a puncher with the diameter of 18mm, the leaf discs are soaked in the liquid medicine to be tested for 10 seconds, then the leaf discs are placed into a culture dish (with the diameter of 90 mm) filled with moisturizing filter paper, 5 leaf discs are placed into each dish, after the leaf discs are naturally dried, 3-year larvae of plutella xylostella starved for 4 hours are selected into the culture dish, each dish is not lower than 10 heads, 4 times of repetition are carried out, after the treatment is finished, a dish cover is covered, and the leaf discs are placed into an observation chamber for culture.
5 data investigation and statistical analysis
5.1 investigation time and method
After 72 hours, the death condition of the test insects is checked and recorded, and the death judgment standard of the test insects is that the test insects are gently contacted by forceps and have no response, so that the test insects are dead.
5.2 method for evaluating synergy
And (3) solving the co-toxicity coefficient (CTC) of each compounding combination by adopting a Sun & Johnson (1960) co-toxicity coefficient method according to the indoor biological assay criterion NY/T1154.7-2006 of the pesticide. CTC is less than or equal to 80 and is antagonistic, CTC 80 is additive, CTC 120 is synergistic, CTC is greater than or equal to 120. The co-toxicity coefficient calculation formula is as follows:
drug combination Theory Toxicity Index (TTI) =toxicity index of agent a×percent (%) of agent a in the combination+toxicity index of agent b×percent (%)
6 experimental results
The toxicity measurement results of chlorantraniliprole and tolfenpyrad mixed in the proportions of 3:2, 1:1, 2:3, 1:2 and 1:3 on cabbage diamondback moth are shown in Table 1. From the following componentsThe results show that the chlorantraniliprole and the tolfenpyrad are compounded according to the proportion of 5, except 18:7, and the LC of the chlorantraniliprole and tolfenpyrad has synergistic effect 50 The values are 1.06, 1.07, 1.10, 1.44 and 1.81mg/L, respectively, and the co-toxicity coefficients are 106.35, 124.33, 147.51, 132.01 and 133.70, respectively, wherein the synergy at 2:3 is most significant.
TABLE 1 toxicity measurement results of Chlorantraniliprole and tolfenpyrad mixture on cabbage plutella xylostella
The indoor test result shows that chlorantraniliprole and tolfenpyrad are mixed in the proportion of 3:2, 1:1, 2:3, 1:2 and 1:3, and the synergistic effect is obvious to plutella xylostella except 3:2, wherein the synergistic effect is most obvious in the proportion of 2:3. Therefore, the optimal ratio of chlorantraniliprole to tolfenpyrad can be seen as 2:3 only from the synergistic toxicity comparison.
Application example three: example 1 field efficacy test for controlling cabbage Plutella xylostella
1 purpose of test
The 25% chlorantraniliprole-tolfenpyrad suspending agent developed by the applicant is verified to have the control effect on cabbage plutella xylostella and the safety on cabbage, the field use dosage and the application technology are defined, and a scientific basis is provided for pesticide registration.
2 basis of test
The test complies with the pesticide registration test quality management Specification, the agricultural industry standard pesticide registration field efficacy test quality management Specification (NY/T2885-2016) and the pesticide field efficacy test criterion (one): the pesticide control of lepidoptera larva of crucifer (GB/T17980.13-2000) and the standard operation procedure of pesticide control of lepidoptera larva of crucifer (SXAU-SOP-I-014) of the test unit SOP are carried out.
3 experiment site
The test was set up in Qingxu county, shanxi province.
4 selection of test subjects, crops and varieties
Test object: cabbage plutella xylostella;
test crop: cabbage, variety of Zhonggan No. 28, is transplanted in the field 5 months 5 days of 2021. The previous crop in the test field is cabbage.
5 test design and arrangement
5.1 dosage and numbering of the medicament
TABLE 2 test design of reagents for test
5.2 times and times of application
The medicine is applied once in 2021 at 6-21 days, and is started before the young larvae of plutella xylostella are contained, the medicine is weighed according to the medicine application amount required by each treatment, and the medicine is mixed with water for conventional spraying, so that the spraying is required to be uniform and consistent, and the spraying is not repeated and is not leaked. The blank control was sprayed with water.
5.3 usage Capacity
50 liters of pesticide liquid is sprayed per mu, and the spraying liquid amount per hectare is 750 liters.
5.4 investigation time and times
Five spots were investigated randomly per cell, five plants per spot, and the whole plants were investigated.
First investigation: the number of insect population was investigated and recorded before administration on day 21, 6, 2021.
Second investigation: the number of residual worms was recorded 1 day after 2021, 6 and 22 days after the drug.
Second investigation: the number of residual worms was recorded 3 days after the drug, 24 days 6 in 2021.
Third investigation: the number of residual worms was recorded 7 days after 2021, 6 and 28 days after the drug.
5.5 method for calculating efficacy
Wherein: PT (PT) 0 -number of pre-drug insects in the drug treatment zone;
PT 1 -number of insects after the drug treatment zone;
CK 0 -number of pre-drug insects in the blank control area;
CK 1-number of insects after drug administration in the blank control area;
6 experimental results
TABLE 3 example 1 results of field efficacy test for controlling cabbage Plutella xylostella
The experimental results show that: 1 day after the medicine, the control effects on cabbage moth are 49.42%, 57.69% and 65.57% respectively when the dosage of the 25% chlorantraniliprole-tolfenpyrad suspending agent for the test object in the embodiment 1 is 10 g/mu, 15 g/mu and 20 g/mu; the control agent 5% chlorantraniliprole suspending agent 55 g/mu and 15% tolfenpyrad suspending agent 50 g/mu have the control effect of 51.978% and 56.098%.
3 days after the medicine, when the dosage of the 25% chlorantraniliprole-tolfenpyrad suspending agent serving as a test medicament is 10 g/mu, 15 g/mu and 20 g/mu, the control effect on cabbage plutella xylostella is 66.78%, 73.71% and 80.59% respectively; the control agent 5% chlorantraniliprole suspending agent 55 g/mu and 15% tolfenpyrad suspending agent 50 g/mu have the control effect of 69.83% and 72.96%.
7 days after the medicine, when the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, 15 g/mu and 20 g/mu, the control effect on cabbage plutella xylostella is 82.22%, 87.97% and 91.38% respectively; the control agent 5% chlorantraniliprole suspending agent 55 g/mu and 15% tolfenpyrad suspending agent 50 g/mu have the control effect of 83.58% and 85.01%.
The test results are analyzed by adopting a DMRT method, and the analysis shows that:
the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 20 g/mu, the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, 15 g/mu, the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu and 15% tolfenpyrad suspending agent is 50 g/mu, and the prevention effect difference on cabbage moth reaches a very significant level; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 15 g/mu, the dosage of the control medicament 15% tolfenpyrad suspending agent is 50 g/mu, and the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, so that the difference of the prevention effect on cabbage diamond back moth is extremely remarkable; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 15 g/mu and the dosage of the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu, so that the difference of the prevention effect on cabbage plutella xylostella reaches a remarkable level; the dosage of the test medicament 25% chlorantraniliprole suspending agent is 15 g/mu and the dosage of the control medicament 15% tolfenpyrad suspending agent is 50 g/mu, and the dosage of the test medicament 25% chlorantraniliprole suspending agent is 10 g/mu and the dosage of the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu, so that the prevention effect difference on cabbage moth does not reach a significant level.
The dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 20 g/mu, the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, 15 g/mu, the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu and 15% tolfenpyrad suspending agent is 50 g/mu, and the prevention effect difference on cabbage moth reaches a very significant level; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 15 g/mu, the dosage of the control medicament 15% tolfenpyrad suspending agent is 50 g/mu, and the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, so that the difference of the prevention effect on cabbage diamond back moth is extremely remarkable; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 15 g/mu and the dosage of the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu, so that the difference of the prevention effect on cabbage plutella xylostella reaches a remarkable level; the dosage of the test medicament 25% chlorantraniliprole suspending agent is 15 g/mu and the dosage of the control medicament 15% tolfenpyrad suspending agent is 50 g/mu, and the dosage of the test medicament 25% chlorantraniliprole suspending agent is 10 g/mu and the dosage of the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu, so that the prevention effect difference on cabbage moth does not reach a significant level.
The dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 20 g/mu and the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, and the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu and 15% tolfenpyrad suspending agent is 50 g/mu, so that the prevention effect difference on cabbage moth is extremely remarkable; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 15 g/mu, and the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is between 10 g/mu and the control medicament 5% chlorantraniliprole suspending agent 55 g/mu, so that the difference of the prevention effect on cabbage diamond back moth is extremely remarkable; the dosage of the test medicament 25% chlorantraniliprole suspending agent is 20 g/mu and the dosage of the test medicament 25% chlorantraniliprole suspending agent is 15 g/mu, and the dosage of the test medicament 25% chlorantraniliprole suspending agent is 15 g/mu and the dosage of the control medicament 15% chlorantraniliprole suspending agent is 50 g/mu, so that the difference of the prevention effect on cabbage moth is remarkable; the dosage of the test medicament 25% chlorantraniliprole-tolfenpyrad suspending agent is 10 g/mu, the control medicament 5% chlorantraniliprole suspending agent is 55 g/mu and the 15% tolfenpyrad suspending agent is 50 g/mu, and the prevention effect difference on cabbage plutella xylostella does not reach a significant level.
In the whole test process, no phytotoxicity is found to be generated on leaves and plants of the tested crops by applying the test drugs, and no adverse effect is found to be generated on the surrounding environment.
Application example four: example 2 field efficacy test for controlling cabbage Plutella xylostella
The test purpose, the test basis and the test agent are the same as those in the third application example.
1 experiment site
Experiments were arranged in the Wuming region of Guangxi nan Ning.
2 selection of test subjects, crops and varieties
Test object: cabbage plutella xylostella;
the cabbage is of the type of Jingfeng No. one, 3500 plants/mu, is in the growing period and has good plant growth. The fertilizer and water management is consistent, and the growth vigor of the cabbage is uniform.
3 times and times of application
The test was applied 1 time for 2021, 10 months and 18 days, and the application time was larval development stage.
4 Water consumption
Spraying method, adding water 900L/hectare.
5 investigation time, times and method
3 times of investigation are carried out on 3 days and 9 days (namely, 18 days of 10 months, 21 days of 10 months and 27 days of 10 months) before and after the medicine.
The insect population density investigation is carried out on 3 rd day and 9 th day before and after the drug administration, 10 points are investigated in each district, and the number of the living larvae of the plutella xylostella in different ages on the whole cabbage is fixedly investigated at each point.
6 calculation of efficacy
7 experimental results
TABLE 4 example 2 field control Effect-control Effect on cabbage Plutella xylostella
Note that lowercase letters indicate differences between treatments at the 0.05 level and uppercase letters indicate differences between treatments at the 0.01 level.
The experimental results show that: the 25% chlorantraniliprole-tolfenpyrad suspending agent for the test object of the example 2 is used for preventing and controlling cabbage moth, 3 days after the drug, the prevention and treatment effects of 25% chlorantraniliprole-tolfenpyrad suspending agent 10, 15 and 20 g/mu on cabbage moth are respectively as follows: 75.34%, 79.34%, 82.90%; the control effect of 55 g/mu of chlorantraniliprole suspending agent and 50 g/mu of 15% tolfenpyrad suspending agent on cabbage moth is as follows: 77.90% and 77.43%. The test result is tested and analyzed by a DMRT method, the 25% chlorantraniliprole-tolfenpyrad suspending agent of the tested object is low, and the control effect of concentration treatment (15 g/mu and 20 g/mu) is equivalent to that of two control objects; the control effect of the tested object 25% chlorantraniliprole-tolfenpyrad suspending agent treated with high concentration (20 g/mu) is higher than that of two control objects, and the difference is obvious.
The prevention and treatment effects of the 25% chlorantraniliprole-tolfenpyrad suspending agent for the tested object on cabbage moth after 9 days of medicine treatment are respectively as follows: 79.60, 83.68%, 86.30%; the control effect of 55 g/mu of chlorantraniliprole suspending agent and 50 g/mu of 15% tolfenpyrad suspending agent on cabbage moth is as follows: 83.62% and 79.09%. The test result is checked and analyzed by a DMRT method, and the control effect of the 25% chlorantraniliprole-tolfenpyrad suspending agent low-concentration treatment (10 g/mu) of the test object is equivalent to that of two control objects; the control effect of the high-concentration treatment (15 g/mu) in the 25% chlorantraniliprole-tolfenpyrad suspending agent of the tested object is equivalent to that of the control object treated by 55 g/mu of the 5% chlorantraniliprole suspending agent, but the control object is higher than that of the control object treated by 50 g/mu of the 15% chlorantraniliprole suspending agent, and the difference is obvious.
Application example five: examples 1 and 2 environmental impact measurement experiments
I entrust third party company to carry out 10 tests such as a bee acute oral toxicity test, a bee acute contact toxicity test, a bird acute oral toxicity test, a fish acute toxicity test, a silkworm acute toxicity test, a daphnia acute activity inhibition test, an algae growth inhibition test, an earthworm acute toxicity test, a natural enemy trichogramma acute toxicity test, a natural enemy ladybug acute contact toxicity test and the like on the examples 1-2, wherein the test results are as follows:
1) The bee acute oral toxicity test shows that the toxicity level is low.
2) Bee acute contact toxicity test, the toxicity level is low.
3) Acute oral toxicity test of birds, the toxicity grade is low.
4) Acute toxicity test of fish, the toxicity grade is low.
5) The acute toxicity test of silkworm shows that the toxicity grade is low.
6) The daphnia acute activity inhibition test has low toxicity level.
7) Algae growth inhibition test, toxicity grade is low toxicity.
8) Acute toxicity test of earthworm, the toxicity grade is slightly toxic.
9) The natural enemy trichogramma acute toxicity test is low in risk.
10 Natural enemy ladybug acute contact toxicity test, low risk.
Application example six: examples 1-2 acute toxicology assay experiments
I delegate the third party detection mechanism to conduct acute toxicity test on the embodiment 1-2, and the test result is as follows:
1) The toxicity grade of the acute oral toxicity test of the rat is low.
2) Acute percutaneous toxicity test of rats, the toxicity grade is low.
3) The eye irritation test of rabbits shows no irritation.
4) Skin irritation test, no irritation.
5) Skin sensitization test. The experimental animal is guinea pig; sensitization intensity is zero.
The foregoing is a further detailed description of the invention in connection with the preferred embodiments, and it is not intended that the invention be limited to the specific embodiments described. It will be apparent to those skilled in the art that several simple deductions or substitutions may be made without departing from the spirit of the invention, and these should be considered to be within the scope of the invention.
Claims (7)
1. A preparation method and application of a nanometer suspending agent are characterized in that: the nanometer suspending agent comprises chlorantraniliprole, tolfenpyrad, dispersing agent, wetting agent, defoaming agent, thickening agent and water; wherein the weight ratio of chlorantraniliprole to tolfenpyrad is 1:1-1:3.
2. The method of manufacturing according to claim 1, characterized in that: the ratio of chlorantraniliprole to tolfenpyrad is 2:3.
3. The preparation method according to claim 1 or 2, characterized in that: the total content of chlorantraniliprole and tolfenpyrad is 10% -50%.
4. A method of preparation according to claim 3, characterized in that: the total content of chlorantraniliprole and tolfenpyrad is 25%.
5. The method of manufacturing according to claim 1, characterized in that: firstly, putting water, an auxiliary agent, chlorantraniliprole and tolfenpyrad raw material into a stirring tank for high-speed shearing, and forming primary dispersion after full dispersion; then the slurry is conveyed into a sand mill by a diaphragm pump to be crushed, the sand milling feeding speed is regulated to ensure that the sand milling fineness is controlled to be 0.1-1 mu m, the slurry is finely ground by a rod pin type sand mill, the grain diameter is controlled to be 100-500 nanometers, and the grain size is confirmed to meet the requirement; and finally, conveying the slurry to a preparation kettle, adding a thickening agent and a defoaming agent, adjusting the viscosity of the materials, sampling, and performing quality detection to obtain a finished product.
6. The use according to claim 1, characterized in that: the nanometer suspending agent is used for preventing and controlling cabbage plutella xylostella.
7. The use according to claim 6, characterized in that: the dosage of the active ingredients of the nanometer suspending agent is 37.5-75 g/hectare.
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