CN103329925B - Water dispersible granule of thiamethoxam and pymetrozine composite pesticide and preparation method thereof - Google Patents
Water dispersible granule of thiamethoxam and pymetrozine composite pesticide and preparation method thereof Download PDFInfo
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- CN103329925B CN103329925B CN201310291974.5A CN201310291974A CN103329925B CN 103329925 B CN103329925 B CN 103329925B CN 201310291974 A CN201310291974 A CN 201310291974A CN 103329925 B CN103329925 B CN 103329925B
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Abstract
The invention relates to the technical field of pesticide for controlling rice planthoppers, in particular to a water dispersible granule of thiamethoxam and pymetrozine composite pesticide and a preparation method of the water dispersible granule. The water dispersible granule is prepared by the following ingredients in parts by weight: 15 parts of thiamethoxam, 60 parts of pymetrozine, 15 parts of assistant, 10 parts of filling and less than 5 parts of water. The water dispersible granule of the thiamethoxam and pymetrozine composite pesticide is obviously superior to products prepared according to other proportions in wetting time, suspensibility, persistent foamability, thermal stability and the like. Experiments verify that a cotoxicity coefficient reaches 200.2, and the granule falls in an obvious synergistic action scope. Prepared water dispersible granule insecticide has better systematic and contact actions, damages a normal nervous system of an insect, kills the insect relatively quickly, is longer in lasting period, and has a good effect of controlling the rice planthoppers. The granule is safe to flowers, and free from hazards, and basically has no influence on beneficial organisms such as natural enemies.
Description
Technical field
The present invention relates to rice fulgorid and prevent and treat technical field of pesticide, specifically relate to water dispersible granules of a kind of Diacloden and pymetrozine composite pesticide and preparation method thereof.
Background technology
Diacloden, Universal Chinese character name Acker Thailand, chemistry 3-(the chloro-1,3-thiazoles-5-of 2-ylmethyl)-5-methyl isophthalic acid by name, 3,5-oxadiazines-4-base fork (nitro) amine, belong to the insecticide of high-efficiency low-toxicity, can effectively prevent and treat Lepidoptera, coleoptera, thrips insect, as various aphids, leafhopper, aleyrodid, plant hopper etc., control of insect is difficult for developing immunity to drugs, belongs to environment amenable insecticide.
Pymetrozine, its chemistry (E)-4 by name, 5-dihydro-6-methyl-4-(3-pyridine methylene amino)-1,2,4-triazine-3(2H)-one, can effectively prevent the various pests such as section, Delphacidae, Aleyrodidae, Cicadellidae that eliminate aphis, as cotten aphid, black peach aphid, small brown rice planthopper etc., and control of insect is difficult for developing immunity to drugs, belongs to environment amenable insecticide.
At present, existing for preventing and treating the composite pesticide that contains Diacloden and pymetrozine of rice fulgorid, for example Chinese patent " CN101810187A " discloses a kind of " containing the composition pesticide of Diacloden and pymetrozine ", wherein the weight ratio of Diacloden and pymetrozine is 9:1 to 1:9, and make the various formulations that are suitable for spraying, meanwhile, the preferred 1:1 component proportion of this composition pesticide makes the synergistic effect of its agricultural chemicals the most remarkable.
Inventor is through long term test checking, and this composition pesticide exists following defect:
1), by disclosed several concrete proportionings in said composition are tested, discovery cannot realize the good control efficiency to rice fulgorid.
2), for the disclosed several formulations of said composition, find all to exist the defect of different problems through verification experimental verification.For example, wetting powder easily causes and product bonding is difficult for dispersion suspension in water, or stops up shower nozzle, and the phenomenon such as reason precipitation in sprayer causes and sprays irregularly, easily makes that plant is local produces poisoning.Pulvis in use, the particulate that diameter is less than 10 microns, because being subject to the impact of ground air-flow, easily drift, waste dose, also can cause environmental pollution, affects people healthy.
3), composite problem, measure and find by the disclosed several concrete proportionings of this composition pesticide being carried out to the test of virulence test, heat storage stability and mixture co-toxicity coefficient, cannot reach the notable synergistic effect of two kinds of medicaments, rice fulgorid control efficiency is unsatisfactory.
Summary of the invention
One of object of the present invention is to provide the water dispersible granules of a kind of Diacloden and pymetrozine composite pesticide, and this dosage form of water dispersible granule is reasonable in design, good to rice fulgorid control efficiency, and can realize the notable synergistic effect of Diacloden and pymetrozine.
For achieving the above object, the present invention has adopted following technical scheme:
A water dispersible granules for Diacloden and pymetrozine composite pesticide, this water dispersible granules is made up of following component according to weight portion:
Diacloden: 15 parts;
Pymetrozine: 60 parts;
Auxiliary agent: 15 parts;
Filler: 10 parts;
Water: no more than 5 parts.
Meanwhile, the present invention can also be able to further realization by the following technical programs:
Preferably, described auxiliary agent is that phenethyl phenol polyoxyethylene poly-oxygen propylene aether and fatty alcohol-polyoxyethylene ether are mixed according to weight ratio 1:1.
Preferably, described filler is one or more the mixture in kaolin, diatomite and precipitated calcium carbonate.
The water dispersible granules of Diacloden of the present invention and pymetrozine composite pesticide, its beneficial effect shows:
1) water dispersible granules that, prepared by the present invention is all obviously better than the prepared product of other proportionings at aspects such as wetting time, suspensibility, lasting foaming characteristic and heat storage stabilities.
2), by experiment checking, the co-toxicity coefficient when mixed with 1:4 proportioning with Diacloden and pymetrozine reaches 200.2, belong to notable synergistic sphere of action, and the mixed preparation of other proportioning is summation action, cannot realize the synergistic effect of two kinds of medicaments.
3), by experiment checking, Diacloden and pymetrozine, according to the compounded water dispersible granule insecticide of the weight ratio of 1:4, have stronger interior suction and action of contace poison, destroy the normal nervous system of insect, desinsection is knocked down speed, and the lasting period is longer, prevents and treats rice hoppers effect better.
4), by experiment checking, water dispersible granules of the present invention under test dose to flowers safety, without poisoning occur, on the beneficial organisms such as natural enemy substantially without affect.
The preparation method who another object of the present invention is to the water dispersible granules that a kind of Diacloden and pymetrozine composite pesticide are provided, mixes Diacloden, pymetrozine, auxiliary agent and filler, coarse crushing in advance, then carry out air-flow crushing or ultramicro grinding; Add water to carry out mixing granulation, detect the moisture percentage by weight of water dispersible granules not higher than 3%, particle diameter is controlled at 420 μ m～1680 μ m.
The preparation method of the water dispersible granules of Diacloden of the present invention and pymetrozine composite pesticide, preparation technology is comparatively easy, is easy to suitability for industrialized production.
Embodiment
Below optimal way of the present invention is described in further detail.
One, the selection of raw material
1., the former medicine of Diacloden, Shandong United Pesticide Industry Co., Ltd. provides, registration card number: PD20121633, PD20121678, former medicine content 98%, toxicity rank: belong to low wait poison.
The key technical indexes, impurity title and content: acidity is (with H
2sO
4meter) :≤0.5%; Moisture :≤1.0%; Acetone insoluble matter :≤0.5%.
Main physical and chemical: former medicine outward appearance is white crystalline powder, pH is 7～11.Fusing point: 139.1 ℃, vapour pressure: 6.6 × 10
-9pa (20 ℃), solvability (25 ℃, g/L): water 4.1, acetone 48, ethyl acetate 7.0, methyl alcohol 13, carrene 110, hexane >1mg/L, octanol 620mg/L, toluene 680mg/L.Preparation.
2., the former medicine of pymetrozine, Anhui Yangzi Chemical Industry Co., Ltd. provides, registration card number: PD20121678, former medicine content 95%, toxicity rank: belong to low wait poison.
The key technical indexes, impurity title and content: acidity is (with H
2sO
4meter) :≤0.5%; Moisture :≤1.0%; Acetone insoluble matter :≤0.5%.
Main physical and chemical: former medicine outward appearance is white or faint yellow solid powder, 234 ℃ of fusing points, vapour pressure 9.7 × 10
-3pa (20 ℃), solvability (g/L, 20 ℃): water 0.27, ethanol 2.25, n-hexane <0.01.Stable to photo-thermal, under strong alkaline condition, there is certain decomposition.
3., phenethyl phenol polyoxyethylene poly-oxygen propylene aether and fatty alcohol-polyoxyethylene ether, Nanjing Teva-Chem. Co., Ltd. provides; Kaolin, diatomite and precipitated calcium carbonate, Tianjin Supure Science and Technology Co., Ltd. provides.
Testing result, the heat storage stability result of the test of all technical of the prepared water dispersible granules of two, the preparation of the water dispersible granules of Diacloden and pymetrozine composite pesticide, and each embodiment.
Embodiment 1
Diacloden pymetrozine water dispersing granule, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Diacloden | 15 |
| Pymetrozine | 60 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7.5 |
| Fatty alcohol-polyoxyethylene ether | 7.5 |
| Precipitated calcium carbonate | 10 |
| Water | 3 |
Preparation method: Diacloden, pymetrozine, auxiliary agent and filler are mixed, coarse crushing in advance, then carry out air-flow crushing or ultramicro grinding (granularity of pulverizing is as the criterion with the particle size range that meets finished product and controlled).Add water (in actual production, the addition of water is as the criterion with the moisture requirement that meets finished product and controlled) to carry out mixing granulation.The moisture percentage by weight of made water dispersible granules is 1.8%, and particle diameter is 420 μ m～1680 μ m.
Embodiment 2
Diacloden pymetrozine water dispersing granule, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Diacloden | 15.3 |
| Pymetrozine | 61.5 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7 |
| Fatty alcohol-polyoxyethylene ether | 7 |
| Kaolin | 9.2 |
| Water | 2.5 |
Preparation method is with embodiment 1, and the moisture percentage by weight of made water dispersible granules is 1.6%, and particle diameter is 420 μ m～1680 μ m.
Embodiment 3
Diacloden pymetrozine water dispersing granule, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Diacloden | 14.7 |
| Pymetrozine | 59.5 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7.5 |
| Fatty alcohol-polyoxyethylene ether | 7.5 |
| Diatomite | 10.8 |
| Water | 3 |
Preparation method is with embodiment 1, and the moisture percentage by weight of made water dispersible granules is 1.8%, and particle diameter is 420 μ m～1680 μ m.
Embodiment 4
Diacloden pymetrozine water dispersing granule, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Diacloden | 15.2 |
| Pymetrozine | 59.8 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 7.5 |
| Fatty alcohol-polyoxyethylene ether | 7.5 |
| Precipitated calcium carbonate | 10 |
| Water | 3 |
Preparation method is with embodiment 1, and the moisture percentage by weight of made water dispersible granules is 1.8%, and particle diameter is 420 μ m～1680 μ m.
Embodiment 5
Diacloden pymetrozine water dispersing granule, each component and weight proportion thereof are as follows:
| Composition | Weight portion |
| Diacloden | 14.8 |
| Pymetrozine | 61.4 |
| Phenethyl phenol polyoxyethylene poly-oxygen propylene aether | 6.5 |
| Fatty alcohol-polyoxyethylene ether | 6.5 |
| Diatomite | 10.8 |
| Water | 3 |
Preparation method is with embodiment 1, and the moisture percentage by weight of made water dispersible granules is 1.8%, and particle diameter is 420 μ m～1680 μ m.
The Diacloden pymetrozine water dispersing granule that embodiment 1～5 is prepared, the testing result of product all technical is as shown in table 1, and product heat storage stability result of the test is as shown in table 2.
The testing result of 5 embodiment preparing product all technicals of table 1
5 embodiment preparing product heat storage stability result of the tests of table 2
Can find out by table 1 and 2, product prepared by embodiment 1 is all obviously better than the prepared product of other embodiment at aspects such as wetting time, suspensibility, lasting foaming characteristic and heat storage stabilities.
Three, toxicology test
1. rat acute Oral toxicity test:
Female male SD rat acute per os LD
50all be greater than 5000mg/kg b.wt..This sample belongs to hypotoxicity to the toxicity of female male SD rat.
2. rat acute percutaneous toxicity test:
Female male SD rat acute is through skin LD
50value is all greater than 2000mg/kg b.wt..This sample all belongs to the toxicity such as low to female male SD rat.
3. rat acute toxicity on inhalation test:
Female male SD rat acute sucks LD
50all be greater than 2000mg/m3.This sample all belongs to the toxicity such as low to female male SD rat.
4. guinea pig skin irritant test:
Skin irritatin mean scores is 0, and the detected district of cavy has no any skin reaction, and this sample is to guinea pig skin nonirritant.
5. Rabbits with Acute eye irritation test:
The former medicine of submitted sample is 3 to rabbit eye irritation score index, and average eye irritation is 0 (after 48h), and it is normal that 48h recovers, to eye nonirritant.
6. guinea pig skin allergy test
Adopt partial closure to be coated with pico farad, detection zone has no any skin reaction, sensitization rate (%)=0, and according to sensitization strength grading standard, this sample belongs to weak sensitizer.
Four, indoor virulence test
1, formula Design
According to weight ratios different between Diacloden and pymetrozine, be divided into successively totally 6 groups of 0:10,10:0,2:8,4:6,6:4,8:2.
2, for examination insect
Rice fulgorid is random acquisition rice fulgorid nymph from Guai Gang village, little Miao town, Feixi County, Hefei City paddy field, selects and grows normally, and it is relatively consistent that polypide enlivens size, and the individual nymph that vitality is strong does toxicity test examination worm.
3, assay method
Quantitatively take after the dilution of former medicine by than row configuration mixture.First medicament is made to mother liquor take acetone as solvent, be stored in refrigerator for subsequent use.With mother liquor acetone diluted, medicament is designed to each series concentration.Rice fulgorid is put into culture dish (1 ∕ culture dish), with micro intravenous drip instrument by liquid drop in the rice fulgorid chest back side.Before formal mensuration, first carry out the preliminary experiment of measures range mensuration.When mensuration, each concentration is processed 20 larvas, and makes blank with acetone.Check result cultivate 24 hours in 26 ℃ of insulating boxs after.Calculate lethality according to the dead borer population of total borer population, proofread and correct by contrast lethality.Carry out linear regression with lethality value and dosage logarithm, calculate LD
50value, calculates co-toxicity coefficient (C.T.C)
4, toxicity test result
1., the Diacloden virulence to rice hoppers larva mixed with pymetrozine
Diacloden the results are shown in Table 3 with pymetrozine not to be listed as on year-on-year basis the mixed toxicity test to rice hoppers larva.
Table 3 Diacloden indoor biometrics virulence mixed with pymetrozine
Can find out by table 3, in each determined different proportionings, the highest with the virulence of 1:4, LD
50it is 3.40411/; The virulence of 4:6 is taken second place, LD
50it is 3.83233/; Minimum is 6:4, LD
50it is 5.66531/.
2., the Diacloden synergy reaction mixed with pymetrozine
The synergy reaction of two or more pharmacy mix represents with co-toxicity coefficient (C.T.C), synergy reaction is divided into: antagonism (C.T.C is less than 370), summation action (C.T.C is between 70 and 150) and synergistic effect (C.T.C is greater than 150), its testing result of notable synergistic effect (C.T.C is greater than 200) is in table 4.
The synergy reaction that table 4 Diacloden is mixed with pymetrozine
Can find out by table 4, in 4 kinds of determined mixed preparations, the co-toxicity coefficient when mixed with 1:4 proportioning with Diacloden and pymetrozine reaches 200.2, belong to notable synergistic sphere of action, and the mixed preparation of other proportioning is summation action.
Known by above-mentioned analysis, Diacloden and pymetrozine, according to the compounded insecticide of the weight ratio of 1:4, have stronger interior suction and action of contace poison, destroy the normal nervous system of insect, desinsection is knocked down speed, and the lasting period is longer, prevents and treats rice hoppers effect better.
Five, rice fulgorid control
Water dispersible granules of the present invention is suitable prevents and treats rice hoppers, ornamental flower aleyrodid, aphid, on producing, has good application value.
Prevent and treat rice hoppers, ornamental flower aleyrodid, aphid, by recommended dose, by the clear water dilution of q.s, even spraying.Per season is used 3 times at most.Test of pesticide effectiveness result shows, all suitable control ornamental flower aphids of 10 grams～20 grams/acre, 112.5 grams～225 grams/ha of this medicament active ingredients or preparation.Because aphid reproduction rate is high, reproduction speed is fast, is preferably in the aphid phase dispenser control of starting, and controls the amount reproduction of aphid population, thereby avoids unnecessary harm and aphis propagation virus disease.Aphid focuses mostly in the flowers tender part of children and the harm of the mature leaf back side, and dispenser should be sprayed evenly thoughtful, and amount of liquid medicine is enough, till flowers plant positive and negative is moistening.When this medicament control in field flowering plant aphid, morning or dispenser are at dusk convenient to medicament and are fully touched target polypide, are beneficial to and give full play to drug effect.A situation arises depending on aphid for flowers dispenser in whole vegetative period control number of times.From this experimental observation to Growth And Decline of Aphids dynamically infer, this medicament occurs aphid, lasting period of hazard boom phase, therefore, aphid occurred, when the hazard boom phase, advise executing for about 10 days 1 control about 10 days.
Under test dose, to flowers safety, occur without poisoning; The beneficial organisms such as natural enemy, substantially without impact, are specially:
1, the acute absorption toxicity of honeybee (48h): LC
50be 2.29 × 10
3mg/L, low toxicity.
2, the acute toxicity of tagging of honeybee (48h): LD
50be 63.28 μ g/ honeybees, low toxicity.
3, bird acute oral toxicity (168h): LD
50>1.00 × 10
3mg/kgbw, low toxicity.
4, fish acute toxicity (96h): LC
50>1.00 × 10
2mg/L, low toxicity.
5, silkworm acute toxicity (96h): LC
50be 2.84 × 10
2mg/L, low toxicity.
6, oophagous trichogrammae acute toxicity (24h): safety coefficient is 0.51, medium risk.
7, earthworm acute toxicity (14d): LC
50>1.00 × 10
2mg/kg dry ground, low toxicity.
8, Daphnia magna acute toxicity (48h): EC
50for 66.88mg/L, low toxicity.
9, scenedesmus obliquus acute toxicity (72h): EC
50be 1.20 × 10
2mg/L, low toxicity.
Above-described embodiment is described the preferred embodiment of the present invention; not scope of the present invention is limited; design under the prerequisite of spirit not departing from the present invention; various distortion and improvement that those of ordinary skills make technical scheme of the present invention, all should fall in the definite protection domain of the claims in the present invention book.
Claims (3)
1. a water dispersible granules for Diacloden and pymetrozine composite pesticide, is characterized in that: this water dispersible granules is made up of following component according to weight portion:
Diacloden: 15 parts;
Pymetrozine: 60 parts;
Auxiliary agent: 15 parts;
Filler: 10 parts;
Water: no more than 5 parts;
Described auxiliary agent is that phenethyl phenol polyoxyethylene poly-oxygen propylene aether and fatty alcohol-polyoxyethylene ether are mixed according to weight ratio 1:1.
2. the water dispersible granules of Diacloden according to claim 1 and pymetrozine composite pesticide, is characterized in that: described filler is one or more the mixture in kaolin, diatomite and precipitated calcium carbonate.
3. a preparation method for the water dispersible granules of Diacloden and pymetrozine composite pesticide as claimed in claim 1 or 2, is characterized in that: Diacloden, pymetrozine, auxiliary agent and filler mixed, and coarse crushing in advance, then carry out air-flow crushing or ultramicro grinding; Add water to carry out mixing granulation, detect the moisture percentage by weight of water dispersible granules not higher than 3%, particle diameter is controlled at 420 μ m～1680 μ m.
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| CN109042678A (en) * | 2018-09-10 | 2018-12-21 | 梁劲松 | A kind of double anti-persistent pesticides of rice |
| CN113712036A (en) * | 2021-08-31 | 2021-11-30 | 山西运城绿康实业有限公司 | Pymetrozine and thiamethoxam compound insecticide and preparation method thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422153A (en) * | 2008-11-13 | 2009-05-06 | 陕西韦尔奇作物保护有限公司 | Insecticidal composition containing pymetrozine |
| CN101569312A (en) * | 2009-06-05 | 2009-11-04 | 贵州大学 | Pesticide compound containing pymetrozine and thiamethoxam, preparation method and application thereof |
| CN101810187A (en) * | 2010-04-01 | 2010-08-25 | 上海悦联化工有限公司 | Pesticide combination containing thiamethoxam and pymetrozine |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101422153A (en) * | 2008-11-13 | 2009-05-06 | 陕西韦尔奇作物保护有限公司 | Insecticidal composition containing pymetrozine |
| CN101569312A (en) * | 2009-06-05 | 2009-11-04 | 贵州大学 | Pesticide compound containing pymetrozine and thiamethoxam, preparation method and application thereof |
| CN101810187A (en) * | 2010-04-01 | 2010-08-25 | 上海悦联化工有限公司 | Pesticide combination containing thiamethoxam and pymetrozine |
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