CN106465724A - Aqueous suspension agent containing imidacloprid and lambda-cyhalothrin and preparation method and application - Google Patents

Aqueous suspension agent containing imidacloprid and lambda-cyhalothrin and preparation method and application Download PDF

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Publication number
CN106465724A
CN106465724A CN201610851826.8A CN201610851826A CN106465724A CN 106465724 A CN106465724 A CN 106465724A CN 201610851826 A CN201610851826 A CN 201610851826A CN 106465724 A CN106465724 A CN 106465724A
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agent
imidacloprid
cyhalothrin
aqueous suspension
lambda
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叶进刚
党建美
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TIANJIN HIGHPOINT PLANT PROTECTION CO Ltd
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TIANJIN HIGHPOINT PLANT PROTECTION CO Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N53/00Biocides, pest repellants or attractants, or plant growth regulators containing cyclopropane carboxylic acids or derivatives thereof
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N51/00Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds having the sequences of atoms O—N—S, X—O—S, N—N—S, O—N—N or O-halogen, regardless of the number of bonds each atom has and with no atom of these sequences forming part of a heterocyclic ring

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  • Life Sciences & Earth Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Dentistry (AREA)
  • Plant Pathology (AREA)
  • Engineering & Computer Science (AREA)
  • Pest Control & Pesticides (AREA)
  • Agronomy & Crop Science (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Dispersion Chemistry (AREA)
  • Toxicology (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of aqueous suspension agent containing imidacloprid and lambda-cyhalothrin and preparation method and application.This suspending agent is mainly made up of active component, auxiliary agent and disperse medium, and wherein active component is made up of nicotinoids ultra high efficiency New-type wide-spectrum insecticide imidacloprid and pyrethroid parasite killing gamma cyhalothrin, and both weight are than for 2:1.The invention also discloses the preparation method of above-mentioned aqueous suspension agent insecticide pesticide;The medicine of the present invention can effectively prevent and treat the diversified economy crop pest such as the fruit such as Citrus and vegetable, Semen Maydiss, Cotton Gossypii, Oryza sativa L., Caulis Sacchari sinensis and mite class, insecticidal spectrum is wide, can be from many aspects to insect synergism, reach the purpose with regard to energy effective control insect with relatively low dosage, drug cost is low, especially kill Cucumber blight effect more preferably, environmentally friendly.

Description

Aqueous suspension agent containing imidacloprid and lambda-cyhalothrin and preparation method and application
Technical field
The invention belongs to pesticides application technical field, be related to a kind of containing imidacloprid and gamma cyhalothrin aqueous suspension agent Preparation and its application on the agricultural pests such as preventing and treating Cucumber blight.
Background technology
Gamma cyhalothrin(Lambda-cyhalothrin)Chemical name:3- (2- chloro- 3,3,3- trifluoro-propenyl)- 2,2- dimethyl cyclopropane carboxylic acids-alpha-cyano -3- phenoxybenzyl ester, are that a kind of fusing point is relatively low(49.2℃)Pyrethroid Insecticide.It is one of insecticidal toxicity highest kind in current pyrethroid, and has insecticidal spectrum extensively, has one to insect Fixed tag, stomach poison function, there is to ovum certain inhibitory action simultaneously, safer to people and animals, but, single for a long time make Form Drug resistance with easy.Gamma cyhalothrin mainly based on cream and two kinds of dosage forms of water and milk, all using organic molten in a large number Agent, there is a problem of polluting environment, remains larger, production and transportation presence a lot of unsafe factors.
Imidacloprid (Imidachloprid), chemical name:1- [(6- chloro-3-pyridyl ylmethyl) -4,5- dihydro-N nitro Sub- imidazolidine -2- base amine), it is a kind of ultra high efficiency anabasine insecticide of brand new, insecticidal mechanism is unique, and insect is had Tag and stomach poison function, and have stronger osmosiss, be a kind of insecticide of high-efficiency broad spectrum lasting period length.Imidacloprid is removed with plan Worm chrysanthemum ester insecticide compounding use, prevention effect projects.For preventing and treating sucking pest and its resistant strain.
Existing patent CN101380023A and CN103858923A disclose a kind of gamma cyhalothrin and imidacloprid Water dispersible granules, the solvent of 5-30% to be used in granulation process(One or more of ethanol, ethyl acetate, methanol etc.), and And want recycling design, complex process, and production link to yet suffer from safety and pollution problem during granulation drying.The present invention Use, greatly reduce drug cost.Due to the rise of current oil price, also rise therewith for the dimethylbenzene in lytic agent Valency, so decreasing the use of the organic solvents such as dimethylbenzene, is conducive to environmental protection, more avoid to agriculture to crop injury.
Content of the invention
The present invention solves degradable, the appearance that low melting point active compound gamma cyhalothrin runs in making aqueous suspension agent A difficult problem for crystallization.
The invention provides the preparation method containing imidacloprid and the pesticide suspension concentrate of gamma cyhalothrin and its Application on preventing and treating Cucumber blight.
For achieving the above object, technology contents disclosed by the invention are as follows:
A kind of pesticide suspension concentrate containing imidacloprid and gamma cyhalothrin is it is characterised in that it is made up of following raw materials:
Imidacloprid 5 ~ 30%,
Gamma cyhalothrin 3 ~ 20%,
Wetting dispersing agent 3.0 ~ 10.0%,
Antifreezing agent 3 ~ 5%,
Preservative 0.1 ~ 0.5%
Defoamer 0.1 ~ 1%
Thickening agent 0.2 ~ 5.0%,
Disperse medium complements to 100%;
Wherein in suspension seed-coating agent, suspension particle diameter is at 1 ~ 5 μm.
Currently preferred suspension seed-coating agent, it is made up of following raw materials according:Imidacloprid 5 ~ 30%, gamma cyhalothrin 3 ~ 20%, wetting dispersing agent 3 ~ 10%, thickening agent 0.2 ~ 5%, antifreezing agent 3 ~ 5%, defoamer 0.3 ~ 1%, preservative 0.1 ~ 0.5%, Water complements to 100%.
Wetting dispersing agent therein is calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, PULLRONIC F68 Block copolymer, polycarboxylate sodium, polyoxyethylene phosphate, polycarboxylate, lignosulfonates, EO-PO block copolymer, wood Quality sulfoacid calcium, phosphate anion dispersant, anion aryl polyoxy alkyl sulfate, EO-PO block copolymer, low HLB One or more of wetting dispersing agents such as value emulsifying agent, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol sodium sulfonate;
Antifreezing agent refers to ethylene glycol, propylene glycol or carbamide;
Preservative refers to sodium benzoate or highly efficiency compositional component S-30;
Thickening agent is white carbon, organobentonite, xanthan rubber powder or aluminium-magnesium silicate;
Defoamer is organic silicon defoamer AF-9903 or organically-modified silane AF-1501;
Disperse medium is water.Its suspension particle diameter is at 2~5 μm.
The presently preferred aqueous suspension agent containing imidacloprid and gamma cyhalothrin it is characterised in that it be by under State raw material composition:
Imidacloprid is 20%, and gamma cyhalothrin is 10%, and remaining is auxiliary agent, and described auxiliary agent refers to 3% polycarboxylate, 3% Polyoxyethylene ether phosphate, 5% antifreezing agent, 0.5% suspending agent, 0.1% preservative, 0.2%PH regulator, 0.15% viscosifier, water Complement to 100% composition.
Invention further provides the preparation method containing imidacloprid and the aqueous suspension agent of gamma cyhalothrin, it is special Levy and be to carry out by the steps:
(1)By load weighted for step 1 active compound imidacloprid and gamma cyhalothrin, wetting dispersing agent, antifreezing agent, preservative, disappear Infusion and water put in reactor, pre-dispersed with high-shear emulsion machine;
(2)Gained slurry is moved into sand milling tank, is passed through cooling water and carries out sand milling, the suspension particle diameter of sand milling to material reaches at 2~5 μm After more than 98%, slurries filtration is standby;
(3)The aqueous solution that thickening agent is configured to 1~2% is added in the slurry after filtration, detects, qualified be into after debugging Product.
Suspension seed-coating agent prepared by the present invention is white flowable suspension, and low temperature, heat storage stability are qualified, heat storage Resolution ratio is less than 5%, and suspensibility is more than 90%, and wet screening test is more than 98%, and the meso-position radius D50 of granule is 2 ~ 5 μm.
The present invention further discloses containing imidacloprid and gamma cyhalothrin aqueous suspension agent in preventing and treating cereal crops, vegetable Application in dish, fruit and vegerable insect pest.Application particularly in terms of preventing and treating fruit tree, vegetable aphid various crop pests.Experiment knot Fruit shows:The 30% chlorine fluorine being provided by Tianjin Han Bang Co., Ltd. the imidacloprid aqueous suspension prepared dose of quick-acting to Cucumber blight All preferable with lasting effect, preventive effect is better than single dose imidacloprid and single dose gamma cyhalothrin is processed, and no poisoning produces.
The further experimentation of the present invention and result are as follows:
Standard is calculated according to co-toxicity, it is antagonism that CTC value is less than 80, and 80 ~ 120 is summation action, is potentiation more than 120 Effect.The co-toxicity coefficient (CTC) of imidacloprid and high-efficient lambda-cyhalothrin compound, between 139.41 ~ 252.78, wherein presses 2:1 During proportioning, CTC is 252.78 to the maximum, and potentiation is more than other and processes.Imidacloprid and gamma cyhalothrin mixture have rationally Property and feasibility.
(One)Formula development is tested:
1. test material and method
1.1 test material
Imidacloprid:White solid powder, active constituent content 96.7%(Commercially available).
Gamma cyhalothrin:White solid powder, active constituent content 95.4%(Commercially available).
Wetting dispersing agent therein is calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, PULLRONIC F68 Block copolymer, polycarboxylate sodium, polyoxyethylene phosphate, polycarboxylate, lignosulfonates, EO-PO block copolymer, wood Quality sulfoacid calcium, phosphate anion dispersant, anion aryl polyoxy alkyl sulfate, EO-PO block copolymer, low HLB One or more of wetting dispersing agents such as value emulsifying agent, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol sodium sulfonate;
Thickening agent:White carbon, organobentonite, xanthan rubber powder or aluminium-magnesium silicate.
Antifreezing agent:Ethylene glycol, glycerol or carbamide.
Defoamer:Defoamer is organic silicon defoamer AF-9903 or organically-modified silane AF-1501.
Preservative:Sodium benzoate or highly efficiency compositional component S-30.
1.2 test apparatuses
Sand mill(0.1L、0.3L、1.5L), laboratory high-speed shearing emulsion machine, NDJ-1 viscometer, PH meter, centrifuge, laser Particles distribution instrument.
1.3 test method
Using wet method sand milling micronizing.According to recipe requirements, the mixing of active compound, auxiliary agent and disperse medium is sized mixing, is cut with high speed Cut mulser pre-dispersed after, by slurry move into sand milling tank, be passed through cooling water and carry out sand milling, after the particle diameter of sand milling to material is qualified, Filter, detect after debugging, the qualified aqueous suspension agent finished product being 30% chlorine fluorine imidacloprid.
The mensure of 1.4 physicochemical properties
The emulsifying dispersivity of aqueous suspension agent, dewatering ability, viscosity, pH value, pourability, cold storage stability, heat storage stability The equal reference of assay method《The formulations of pesticide process book series》(The third edition)In aqueous suspension agent quality standard and the method for inspection carry out, pyrrole Worm quinoline and gamma cyhalothrin content analysis adopt liquid chromatography.
2nd, recipe determination
The selection of 2.1 wetting dispersing agents
General 2 ~ 5 μm of the particle diameter of pesticide suspension concentrate, due to particle diameter very little, the surface free energy of particle is very big, easily inhales between particle Attached cohesion.In order to improve the stability of aqueous suspension agent, generally a certain amount of wetting dispersing agent must be added, in the week of dispersed phase particles Enclose and form firm protecting film, be allowed in storage process not occur to condense and tie bottom phenomenon.There is a small amount of bleed layering, gently shake Dynamic can become stable suspension system, and have good in dispersibility.
Physical and chemical performance according to imidacloprid and gamma cyhalothrin and research experience, we select different moistenings to divide Powder is screened (table 1)
Table 1 wetting dispersing agent Selection experiment(Unit:%)
The selection of 2.2 thickening agents
Viscosity is a key factor of impact suspending agent product bin stability.Viscosity is too little, and product can be caused to put for a long time Put easy layering, caking;Viscosity is too big, and product is difficult to topple over serious wall built-up, affects product dispersibility, brings tired to processing and use Difficult.In order to improve the pourability of product, improve suspensibility and bin stability it must be determined that suitable range of viscosities.For this reason, root According to the development Experience of suspending agent, on the basis of 8# formula, we screen several thickening agents and have carried out stability test, find yellow Preferably, it the results are shown in Table 2 to virgin rubber thickening agent effect.
Knowable to the selection result, formulation flows while with preparation dewatering ability when xanthan rubber powder (0.15%) preferably Property preferably, therefore finally determine xanthan gum as the thickening agent of 30% 30% chlorine fluorine imidacloprid SC, its consumption is 0.15%.
Table 2 thickening agent Selection experiment
The selection of 2.3 antifreezing agents
Pesticide suspension concentrate with water as medium, its formula should be suitable for storing under southern hot conditionss and applying, and And the also storage under north cold area to be considered and application.We have done gradient pair to conventional ethylene glycol, glycerol, carbamide Ratio test, when test finds to make antifreezing agent with glycerol and carbamide, cold storage(-20℃)The no significant change of aqueous suspension agent outward appearance, but Mobility is deteriorated, no significant change during cold ethanediol storage.Therefore, as antifreezing agent, its consumption is 4.0 to this formulation selection ethylene glycol ~ 5.0%.
The selection of 2.4 defoamer
Adopting Wet multi-stage sand milling superfine grinding the production technology of agricultural chemicals suspension agent, the dispersion impeller of high-speed rotation is substantial amounts of sky more Gas is brought into and is dispersed into atomic little bubble, makes suspending agent rapid spatial expansion.These micro-bubbles not only can affect viscosity (stream Dynamic property is deteriorated), measure and pack, and the sand milling efficiency during significant reduction is produced.So, pharmaceutical formulation adds one Quantitative defoamer, and require each component that defoamer must be able to same preparation to have good intermiscibility.This formula is disappeared with organosilicon Infusion AF-9903, is characterized in that defoaming effect is good, good with each group split-phase dissolubility of preparation, and consumption is few, dosage 0.3%, and price is fitted In.
3 30% chlorine fluorine. the determination of imidacloprid aqueous suspension prepared agent prescription and checking
3.1 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of technical specification
Table 3 technical specification
3.2 30% chlorine fluorine. imidacloprid aqueous suspension prepared agent prescription, by testing to the intersection screening of former steps and heat storage stability, obtains Arrive optimal formulation, its formula is as follows:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 3% polycarboxylate, 3% polyoxyethylene ether phosphate, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.3% defoamer AF- 9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, 0.2% glacial acetic acid, water complements to 100%.
The sample prepared by optimal formulation, detects its all technical, its result such as table 4:
Table 4 sample detection result
4. result
(1)Obtain formula as follows:Its formula is as follows:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 3% gathers Carboxylate, 3% polyoxyethylene ether phosphate, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.3% froth breaking Agent AF-9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, 0.2% glacial acetic acid, water complements to 100%.
(2)Through cold storage(0 DEG C, 7 days), heat storage(54 DEG C, 14 days)And alternate freezing and thawing(- 20 DEG C, 16 hours;54 DEG C, 8 hours) Experiment, 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of outward appearance is qualified, favorable dispersibility in water, and it is related that indices all meet suspending agent Standard.
(2) the imidacloprid and high-efficient lambda-cyhalothrin compound synergism test to Cucumber blight
In order to prevent and treat the Cucumber blight in agricultural production, the present invention has been carried out mutually compounding with imidacloprid and gamma cyhalothrin Potentiation research, test is test object using Cucumber blight, and concrete grammar is:
First active compound single dose and each Mixed Pharmacy are arranged 5 variable concentrations gradients(On the basis of preliminary result, test worm is dead Rate of dying is set by geometric progressions in the range of 5% ~ 99%).Test worm Cucumber blight is the Cucumber blight ovum picking up from field, and greenhouse is raised Foster three generations, selects 3 age nymphs of uniformity, carries out indoor potentiation bioassay using Fructus Cucumidis sativi leaf dipping method, often processes 3 weights Multiple, each concentration processes 60, calculates each medicament to the virulence regression equation of Cucumber blight and the lethal concentration of 50 with niqueMin method LC50, with LC50 value according to the abundant method of Sun Yun and according to following equation, calculate mixture spends coefficient together(CTC).If CTC is more than 120, For potentiation;It is antagonism that CTC value is less than 80, and 80 ~ 120 is summation action.
The results are shown in Table 5:
Table 5 imidacloprid and gamma cyhalothrin and its compounding toxicity test to Cucumber blight
Table 6 imidacloprid and gamma cyhalothrin and its compounding co-toxicity effect to Cucumber blight
According to Sun Yunpei system co-toxicity coefficient method, experimental data is carried out process, analysis result shows(It is shown in Table 6):Imidacloprid and height The co-toxicity coefficient (CTC) of effect lambda-cyhalothrin compound between 139.41 ~ 252.78, imidacloprid and high-efficient lambda-cyhalothrin compound When co-toxicity coefficient be all higher than 120, show as potentiation;Wherein press gamma cyhalothrin:Imidacloprid=2.0:During 4.0 proportioning, CTC is Greatly 252.78, potentiation is more than other and processes.Imidacloprid and gamma cyhalothrin mixture have reasonability and feasibility.
Disclosed by the invention containing imidacloprid and gamma cyhalothrin aqueous suspension agent and preparation method and application, and existing Imidacloprid and gamma cyhalothrin produce dosage form the had good effect that compares and be:
(1)Aqueous suspension agent of the present invention using imidacloprid and high-efficient lambda-cyhalothrin compound as effective ingredient, by pyrrole worm Quinoline and two kinds of mechanisms of action of gamma cyhalothrin have the insecticide of larger difference mixture use in appropriate proportions, its parasite killing Effect is substantially better than imidacloprid and gamma cyhalothrin single dose.Suspending agent, with water as disperse medium, will not occur by organic molten The inflammable and drug injury problem that agent produces.Suspending agent has preferable dispersibility and plate-out ability, and suspensibility is high, sticks to plant surface The ability in face is stronger, resistance of rainwater washing against, thus drug effect is notable compared with wettable powder and also relatively more lasting.Gamma cyhalothrin Common dosage forms are mainly cream and aqueous emulsion, change and make the suspending agent that gamma cyhalothrin is compounded with imidacloprid, decrease organic The use of solvent, when using, solves pollution environment, remains higher, production and transportation presence a lot of unsafe factors Problem.
(2)The present invention solve low melting point active compound gamma cyhalothrin make aqueous suspension agent in run into degradable, A difficult problem for crystallization occurs.Simultaneously that gamma cyhalothrin is notable with the effect of imidacloprid compound synergic, solve one-component and kill The deficiency that during worm, drug effect reduces and Drug resistance produces, the dosage reducing pesticide is beneficial to the sustainable development of environment.
(3)The compositionss of the present invention are mainly used in preventing and treating cereal crops, vegetable, the insect in fruit tree, such as aphid, dark greyish green Aphid in the vegetable crops such as worm, aleyrodid etc., especially Fructus Cucumidis sativi.
Brief description
Fig. 1 is pesticide suspension concentrate preparation flow figure.
Specific embodiment
Describe the present invention below by specific embodiment.Unless stated otherwise, technological means used in the present invention It is method known in those skilled in the art.In addition, embodiment is interpreted as illustrative, and the unrestricted present invention Scope, the spirit and scope of the invention are limited only by the claims that follow.To those skilled in the art, without departing substantially from this On the premise of invention spirit and scope, the material component in these embodiments and consumption are carried out various changes or are changed Belong to protection scope of the present invention.The present invention is raw materials used and reagent is commercially available.Such as crude drug imidacloprid, efficient chlorine fluorine cyanogen Chrysanthemum ester active compound is commercially available, polycarboxylate, polyoxyethylene ether phosphate, suspending agent aluminium-magnesium silicate, thickening agent xanthan rubber powder, defoamer AF-9903, antifreeze glycol, glacial acetic acid is commercially available.
Embodiment 1
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 3.0% calcium dodecyl benzene sulfonate, 1.0% alkylaryl polychloroprene polyoxyethylene ether, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.3% Defoamer AF-9903,5.0% antifreeze glycol, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 2
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 2.0% calcium dodecyl benzene sulfonate, 3.0% polyoxyethylene phosphate, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.30% defoamer AF- 9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 3
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 4.0% castor oil polyoxyethylene ether, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.30% defoamer AF-9903,5.0% antifreezing agent second two Alcohol, 0.10% preservative sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 4
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 6.0% castor oil polyoxyethylene ether, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.30% defoamer AF-9903,5.0% antifreezing agent second two Alcohol, 0.10% preservative sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 5
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 1.0% calcium dodecyl benzene sulfonate, 3.0% polychloroprene polyoxyethylene ether, 0.10% suspending agent aluminium-magnesium silicate, 0.20% thickening agent xanthan rubber powder, 0.30% defoamer AF-9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, water complements to 100%.
Embodiment 6
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 5.0% alkylphenol sodium sulfonate, 2.0% EO/PO block polymer, 3.5% organobentonite, 0.30% defoamer AF-9903,5.0% antifreeze glycol, 0.10% prevents Rotten agent sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 7
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 3.0% polychloroprene polyoxyethylene ether, 3.0% polycarboxylate, 0.15% thickening agent xanthan rubber powder, 0.30% defoamer AF-9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
Embodiment 8
Formula forms:20.0% imidacloprid active compound, 10.0% gamma cyhalothrin active compound, 2.0% calcium lignosulfonate, 3.0% Polyoxyethylene phosphate, 3.0% polycarboxylate, 0.50% suspending agent aluminium-magnesium silicate, 0.15% thickening agent xanthan rubber powder, 0.30% disappears Infusion AF-9903,5.0% antifreeze glycol, 0.10% preservative sodium benzoate, 0.20% glacial acetic acid, water complements to 100%.
The preparation method of embodiment 1-8:
(1)By load weighted for step 1 active compound imidacloprid and gamma cyhalothrin, wetting dispersing agent, antifreezing agent, preservative, disappear Infusion and water put in reactor, pre-dispersed with high-shear emulsion machine;
(2)Gained slurry is moved into sand milling tank, is passed through cooling water and carries out sand milling, the suspension particle diameter of sand milling to material reaches at 2~5 μm After more than 98%, slurries filtration is standby;
(3)The aqueous solution that thickening agent is configured to 1~2% is added in the slurry after filtration, detects, qualified be into after debugging Product 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose.
30% chlorine fluorine as obtained by the embodiment of the present invention 8 formula. imidacloprid aqueous suspension prepared dose respectively Jixian Tianjin, Shandong, Chongqing (2014,2015) this four areas carry out efficacy testing, and result is as follows:
30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight field control effectiveness test(Jixian Tianjin)
Experimental condition:Zhuan Cun is helped to change in Jixian, tianjin Municipality Yin Liu town, and for studying thing Fructus Cucumidis sativi, test kind is emerald green No. 6, and each test is little Area's cultivation condition is consistent.
Test sets 6 process, the made medicament of the present invention 30% chlorine fluorine altogether. tri- concentration of imidacloprid SC;Comparison medicament 2.5% is high Effect lambda-cyhalothrin EC;Comparison medicament 10% imidacloprid WP;And clear water comparison.Specifically selected medicament and spraying medicine concentration such as table 7 institute Show.
Table 7 tests selected medicament and spraying medicine concentration
This test sets six process altogether as shown in Table 7, often processes 4 repetitions, totally 24 cell, every cell 25.6, experimental plot Random district's groups arrangement, on June 1st, 2015 disposable medication, amount of liquid medicine 450 liter/hectare during spraying.With Shandong bodyguard's fog machine Tool company limited produces the spraying of " WS-16P " type aerosol apparatus.
Investigation method:Investigate in four times altogether, before dispenser, investigate insect population, each investigation after 1,3,7 days after dispenser once, is remembered Record Aphed population.
Every cell investigates the Aphed population alive on 10 plants of plant of labelling.
Drug effect calculates:Carry out according to the following formula:
Prevention effect(%)=[1- (CK0 borer population × Pt1 borer population)/(CK1 borer population × Pt0 borer population)] × 100
In formula:After CK1--- check plot medicine before the medicine of CK0--- check plot
After Pt1---- treatment region medicine before Pt0--- treatment region medicine
Table 8 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight result of the test
Using the new multipole of Duncan poor (DMRT) method, statistical analysiss are carried out to test data, obtain table 8.
As can be seen from Table 8, after medication 1 day, 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of prevention effect to Cucumber blight with Formulation rate increases and improves, and the preventive effect of three process is respectively 71.76%, 74.58%, 78.69%;The efficient chlorine of comparison medicament 2.5% The preventive effect of flucythrinate cream and 10% imidacloprid wettable powder respective handling is 75.48% and 73.75%.It is anti-that each is processed All there is not significant difference each other in effect.
After medication 3 days, the prevention effect that each is processed is improved, reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose Preventive effect is respectively 85.19%, 90.62%, 92.71%;Comparison medicament 2.5% efficient cyhalothrin emulsifiable concentrate and 10% imidacloprid are wettable Property powder respective handling preventive effect be 88.75% and 90.67%.Significance difference analysis are carried out to this result, result shows, process C is reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose 36 grams/ha(Effective ingredient)In preventive effect, significantly good pretreatment A supplies Reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose 18 grams/ha(Effective ingredient)Outward, the preventive effect that each is processed is each other all not There is significant difference.
After medication 7 days, the prevention effect that each is processed all maintains higher level, reagent agent 30% chlorine fluorine. and imidacloprid water hangs The preventive effect of floating three process of agent is respectively 89.57%, 92.27% and 94.35%;The efficient chlorine fluorine cyanogen of comparison medicament comparison medicament 2.5% The preventive effect of chrysanthemum emulsifiable concentrate and 10% imidacloprid wettable powder respective handling is 91.87% and 89.40%.Significance difference analysis are tied Fruit was with 1 day after medicine.
Result of the test shows:The 30% chlorine fluorine that Tianjin Han Bang Co., Ltd provides. imidacloprid aqueous suspension prepared dose to Huang Melon aphid worm has good prevention effect, Cucumber blight low instar larvae occur the phase use, can effective control Cucumber blight harm, Using dosage is commodity amount 4-8 milliliter/mu(18-36 gram/ha of effective dose)It is advisable.Result of the test refers to table 8.
Embodiment 10
30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight field control effectiveness test(Shandong)
Experimental condition:The good Meng in Shandong Province Qingzhou City Gao Liu town, for studying thing Fructus Cucumidis sativi, test kind is 3966, and each experimental plot plants Training is consistent.
Test sets 6 process, the made medicament of the present invention 30% chlorine fluorine altogether. tri- concentration of imidacloprid SC;Comparison medicament 2.5% is high Effect lambda-cyhalothrin EC;Comparison medicament 35% imidacloprid SC;And clear water comparison.Specifically selected medicament and spraying medicine concentration such as table 9 institute Show.
Table 9 tests selected medicament and spraying medicine concentration
This test sets six process altogether as shown in Table 7, often process 4 times repetition, totally 24 cell, every cell 50, experimental plot with Machine district's groups arrange, on May 4th, 2015 disposable medication, amount of liquid medicine 675 liter/hectare during spraying.
Investigation method:Investigate in four times altogether, before dispenser, investigate insect population, each investigation one after 1,3,7,10 days after dispenser Secondary, record Aphed population.
Every 5 points of samplings of cell, every 5 plants of Fructus Cucumidiss sativi, fixing three for every plant has worm blade, and every cell investigates 25 plants altogether, 75 Blade.All record the Aphed population of survival on labelling cucumber leaves every time.
Drug effect calculates:Carry out according to the following formula:
Revision insect recluced rate(%)=[(Borer population alive after borer population-dispenser alive before dispenser)Borer population alive before/dispenser] * 100
Prevention effect(%)=(Treatment region Revision insect recluced rate-check plot Revision insect recluced rate)/(1- check plot Revision insect recluced rate)×100
Table 10 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight result of the test
Using the new multipole of Duncan poor (DMRT) method, statistical analysiss are carried out to test data, obtain table 10.
As can be seen from Table 10, reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight has preferable effect Really.Medication was investigated after 1 day, 30% chlorine fluorine. the 36 grams/ha of preventing and treatings to Cucumber blight of imidacloprid aqueous suspension prepared dose of effective ingredient consumption Effect is 84.16%, better than 9.375 grams/ha of the preventing and treating of comparison medicament 2.5% efficient cyhalothrin emulsifiable concentrate effective ingredient consumption Effect(73.67%), it is worse than the prevention effect of 21 grams/ha of 35% imidacloprid aqueous suspension prepared dose of effective ingredient consumption of comparison medicament (86.76%);30% chlorine fluorine. the prevention effect of 27 grams/ha of imidacloprid aqueous suspension prepared dose of effective ingredient consumption is 73.99%, and compares Medicament 2.5% efficient cyhalothrin emulsifiable concentrate prevention effect is close, is worse than 35% imidacloprid aqueous suspension prepared dose of effect, and its effective ingredient is used The prevention effect of 18 grams/ha of process of amount is 69.07%, is worse than comparison medicament.
Investigate after medication 3 days, reagent agent 30% chlorine fluorine. 27 grams/ha of imidacloprid aqueous suspension prepared dose of effective ingredient consumption anti- Controlling effect is 90.08%;Better than comparison medicament 2.5% efficient cyhalothrin emulsifiable concentrate prevention effect(72.90%), with comparison medicament 35% imidacloprid aqueous suspension prepared dose of prevention effect(89.33%)Close;The prevention effect of effective ingredient consumption 27-18 gram/ha is 86.04% and 82.66%, better than comparison medicament 2.5% efficient cyhalothrin emulsifiable concentrate, it is worse than comparison medicament 35% imidacloprid aqueous suspension prepared Agent.
Medication was investigated after 7-10 days, reagent agent 30% chlorine fluorine. and imidacloprid aqueous suspension prepared dose of effective ingredient is with 36 grams/ha Prevention effect is 91.61%-91.13%, better than other two pairs of comparison medicament preventive effects(It is respectively 74.64%-73.91% and 90.11%- 89.95%).The prevention effect of its effective ingredient consumption 27-18 gram/ha is 87.99%-83.86%, better than comparison medicament 2.5% Efficient cyhalothrin emulsifiable concentrate, is worse than imidacloprid aqueous suspension prepared dose of comparison medicament 35%.
Result of the test shows:The 30% chlorine fluorine that Tianjin Han Bang Co., Ltd provides. imidacloprid aqueous suspension prepared dose to Huang The quick-acting of melon aphid worm and lasting effect are all preferable, and reagent agent dosage, to Fructus Cucumidis sativi safety, grows to it and has no significant effect.
Technical essential:30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of spraying preventing and treating Cucumber blight using dosage is with effective ingredient 18- 36 grams/ha, preparation consumption 4-8 milliliter/mu is advisable, and spraying will uniformly be advisable completely.Result of the test refers to table 10.
Embodiment 11
30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight field control effectiveness test(Chongqing, 2014)
Experimental condition:Qijiang area of Chongqing City is experimental field and periphery is long-term vegetable field, and for studying thing Fructus Cucumidis sativi, each experimental plot plants Training is consistent.
Test sets 6 process, the made medicament of the present invention 30% chlorine fluorine altogether. tri- concentration of imidacloprid SC;Comparison medicament 20% pyrrole Worm quinoline SL;Comparison medicament 10% gamma cyhalothrin SC;And clear water comparison.Specifically selected medicament and spraying medicine concentration such as table 11 Shown.
Table 11 tests selected medicament and spraying medicine concentration
As shown in table 11 this test sets six process altogether, and often process repeats for 4 times, totally 24 cell, every cell 15, experimental plot with Machine district's groups arrange, on July 4th, 2014 disposable medication, amount of liquid medicine 500 liter/hectare during spraying.
Investigation method:It is divided into 3 investigation, investigate insect population before dispenser, after 2,7 days after dispenser, investigate each labelling strain respectively Upper wingless aphid number.
Using 5 point samplings, 10 plants of every cell labelling, before the medicine, investigate respectively after 2,7 days after medicine aptery in each labelling strain Aphid number.
Drug effect calculates:Carry out according to the following formula:
Revision insect recluced rate(%)=[(Insect population number after insect population number -0 medicine before medicine)Insect population number before/medicine] * 100
Prevention effect(%)=(Treatment region Revision insect recluced rate-check plot Revision insect recluced rate)/(1- check plot Revision insect recluced rate)×100
Table 12 30% chlorine fluorine. the imidacloprid aqueous suspension prepared dose of field control effectiveness test result to Cucumber blight
Using the new multipole of Duncan poor (DMRT) method, statistical analysiss are carried out to test data, obtain table 12.
As can be seen from Table 12, reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose and comparison medicament are respectively processed, to Fructus Cucumidis sativi The field efficacy of aphid.After medication 2 days, survey result is respectively, and 91.36%(36 grams/ha)、86.85%(27 grams/ha)、 78.27%(18 grams/ha)、84.26%(Imidacloprid)With 87.41%(Gamma cyhalothrin);7 days after medicine, each preventive effect processing It respectively is:95.49%th, 92.33%, 84.75%, 90.74% and 92.91%.In each investigation after medicine, test medicine is respectively processed Preventive effect improve with the increase of using dosage, it is higher than two kinds of comparison medicaments that 36 grams/ha of test medicine processes preventive effects;27 grams/ The preventive effect of hectare is suitable with two kinds of comparison medicaments;18 grams/ha process preventive effect and are less than two kinds of comparison medicaments.
The results of analysis of variance patting equal preventive effect everywhere shows, after medicine 2 days consistent with the preventive effect variation tendency of 7 days, and remove Between 27 grams/ha and two kinds single doses of test medicine, between single dose imidacloprid and the process of single dose gamma cyhalothrin, difference is not notable Outward, between remaining process, preventive effect difference all reaches significant level.
Result of the test shows, the 30% chlorine fluorine being provided by Tianjin Han Bang Co., Ltd. imidacloprid aqueous suspension prepared dose to Huang The quick-acting of melon aphid worm and lasting effect are all preferable, and its 3 kinds for the treatment of dosage occur Sheng phase beginning in Cucumber blight, using spraying treatment, There is preferable preventive effect, and no poisoning produces.Advise that the dosage that recommends in Cucumber blight preventing and treating for this product is:Effectively become Component 18-36 mg/kg, amount of formulation is 4-8 gram/acre.
Embodiment 12
30% chlorine fluorine. imidacloprid aqueous suspension prepared dose of preventing and treating Cucumber blight field control effectiveness test(Chongqing, 2015)
Experimental condition:Qijiang area of Chongqing City is experimental field and periphery is long-term vegetable field, and for studying thing Fructus Cucumidis sativi, each experimental plot plants Training is consistent.
Test sets 6 process, the made medicament of the present invention 30% chlorine fluorine altogether. tri- concentration of imidacloprid SC;Comparison medicament 20% pyrrole Worm quinoline SL;Comparison medicament 10% gamma cyhalothrin SC;And clear water comparison.Specifically selected medicament and spraying medicine concentration such as table 13 Shown.
Table 13 tests selected medicament and spraying medicine concentration
As shown in table 13 this test sets six process altogether, and often process repeats for 4 times, totally 24 cell, every cell 30, experimental plot with Machine district's groups arrange, on July 6th, 2015 disposable medication, amount of liquid medicine 500 liter/hectare during spraying.
Investigation method:It is divided into 3 investigation, investigate insect population before dispenser, after 2,7 days after dispenser, investigate each labelling strain respectively Upper wingless aphid number.
Using 5 point samplings, 10 plants of every cell labelling, before the medicine, investigate respectively after 2,7 days after medicine aptery in each labelling strain Aphid number.
Drug effect calculates:Carry out according to the following formula:
Revision insect recluced rate(%)=[(Insect population number after insect population number -0 medicine before medicine)Insect population number before/medicine] * 100
Prevention effect(%)=(Treatment region Revision insect recluced rate-check plot Revision insect recluced rate)/(1- check plot Revision insect recluced rate)×100
Table 14 30% chlorine fluorine. the imidacloprid aqueous suspension prepared dose of field control effectiveness test result to Cucumber blight
Using the new multipole of Duncan poor (DMRT) method, statistical analysiss are carried out to test data, obtain table 14.
As can be seen from Table 14, reagent agent 30% chlorine fluorine. imidacloprid aqueous suspension prepared dose and comparison medicament are respectively processed, to Fructus Cucumidis sativi The field efficacy of aphid.After medication 2 days, survey result is respectively, and 90.17%(36 grams/ha)、85.94%(27 grams/ha)、 75.62%(18 grams/ha)、84.73%(Imidacloprid)With 87.68%(Gamma cyhalothrin);7 days after medicine, each preventive effect processing It respectively is:94.72%th, 90.82%, 82.91%, 88.53% and 90.66%.In each investigation after medicine, test medicine is respectively processed Preventive effect improve with the increase of using dosage, and 7 days after medicine>2 days after medicine.36 grams/ha of test medicine processes preventive effect Two kinds of comparison medicaments;27 grams/ha of preventive effect is suitable with two kinds of comparison medicaments;18 grams/ha process preventive effect and are less than two kinds of comparisons Medicament.
The results of analysis of variance patting equal preventive effect everywhere shows, after medicine 2 days consistent with the preventive effect variation tendency of 7 days, and remove Between 27 grams/ha and two kinds single doses of test medicine, between single dose imidacloprid and the process of single dose gamma cyhalothrin, difference is not notable Outward, between remaining process, preventive effect difference all reaches significant level.
Result of the test shows, the 30% chlorine fluorine being provided by Tianjin Han Bang Co., Ltd. imidacloprid aqueous suspension prepared dose to Huang The quick-acting of melon aphid worm and lasting effect are all preferable, and its 3 kinds for the treatment of dosage occur Sheng phase beginning in Cucumber blight, using spraying treatment, There is preferable preventive effect, and no poisoning produces.This result and this medicament experimental result in 2014 is substantially identical, still advises this product Cucumber blight preventing and treating in the dosage that recommends be:Effective ingredient amount 18-36 mg/kg, amount of formulation is 4-8 gram/acre.
To sum up, the 30% chlorine fluorine that Han Bang Co., Ltd in Tianjin provides. imidacloprid aqueous suspension prepared dose has relatively to Cucumber blight Good quick-acting and lasting effect, and no poisoning produces, it is grown does not affect.There is certain work to crop pests preventing and treating With.

Claims (5)

1. a kind of aqueous suspension agent containing imidacloprid and lambda-cyhalothrin is it is characterised in that it is made up of following raw materials:
Imidacloprid 5 ~ 30%,
Gamma cyhalothrin 3 ~ 20%,
Wetting dispersing agent 3.0 ~ 10.0%,
Antifreezing agent 3 ~ 5%,
Preservative 0.1 ~ 0.5%
Defoamer 0.1 ~ 1%
Thickening agent 0.2 ~ 5.0%,
Disperse medium complements to 100%;
Wetting dispersing agent therein is calcium dodecyl benzene sulfonate, castor oil polyoxyethylene ether, PULLRONIC F68 block Copolymer, polycarboxylate sodium, polyoxyethylene phosphate, polycarboxylate, lignosulfonates, EO-PO block copolymer, lignin Sulfoacid calcium, phosphate anion dispersant, anion aryl polyoxy alkyl sulfate, EO-PO block copolymer, low hlb breast One or more of agent, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol sodium sulfonate, wetting dispersing agent;
Antifreezing agent refers to ethylene glycol, propylene glycol or carbamide;
Preservative refers to sodium benzoate or highly efficiency compositional component S-30;
Thickening agent is white carbon, organobentonite, xanthan rubber powder or aluminium-magnesium silicate;
Defoamer is organic silicon defoamer AF-9903 or organically-modified silane AF-1501;
Disperse medium is water.
2. the aqueous suspension agent containing imidacloprid and lambda-cyhalothrin described in claim 1, its suspension particle diameter is at 2~5 μm.
3. the aqueous suspension agent containing imidacloprid and lambda-cyhalothrin described in claim 1 is it is characterised in that it is by following raw material groups Become:
Imidacloprid is 20%, and gamma cyhalothrin is 10%, and remaining is auxiliary agent, and described auxiliary agent refers to 3% polycarboxylate, 3% Polyoxyethylene ether phosphate, 5% antifreezing agent, 0.5% suspending agent, 0.1% preservative, 0.2%PH regulator, 0.15% viscosifier, water Complement to 100% composition.
4. the preparation method containing imidacloprid and lambda-cyhalothrin aqueous suspension agent described in any one of claim 1-3 is it is characterised in that press The steps is carried out:
(1)By load weighted active compound imidacloprid and gamma cyhalothrin, wetting dispersing agent, antifreezing agent, preservative, defoamer and Water puts in reactor, pre-dispersed with high-shear emulsion machine;
(2)Gained slurry is moved into sand milling tank, is passed through cooling water and carries out sand milling, the suspension particle diameter of sand milling to material reaches at 2~5 μm After more than 98%, slurries filtration is standby;
(3)The aqueous solution that thickening agent is configured to 1~2% is added in the slurry after filtration, detects, qualified be into after debugging Product.
5. described in claim 1 containing imidacloprid and lambda-cyhalothrin aqueous suspension agent in preventing and treating fruit tree, the multiple farming of vegetable aphid The application of thing insect aspect.
CN201610851826.8A 2016-09-26 2016-09-26 Aqueous suspension agent containing imidacloprid and lambda-cyhalothrin and preparation method and application Pending CN106465724A (en)

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CN107258807A (en) * 2017-06-29 2017-10-20 山东大农药业有限公司 A kind of Pesticidal combination containing imidacloprid and gamma cyhalothrin
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Application publication date: 20170301