CN102334478B - Suspoemulsion containing Envidor and preparation methods thereof - Google Patents
Suspoemulsion containing Envidor and preparation methods thereof Download PDFInfo
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- CN102334478B CN102334478B CN201110362700.1A CN201110362700A CN102334478B CN 102334478 B CN102334478 B CN 102334478B CN 201110362700 A CN201110362700 A CN 201110362700A CN 102334478 B CN102334478 B CN 102334478B
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Abstract
The invention provides a suspoemulsion containing Envidor. The suspoemulsion comprises the following components in parts by weight: 1-50 parts of Envidor, 2-10 parts of wetting dispersant, 1-3 parts of antigraining agent, 0.1-2 parts of defoaming agent, 1-25 parts of adhesive, 2-10 parts of emulsifier and 0.1-100 parts of water. The invention also provides preparation methods of the suspoemulsion. One of the preparation methods comprises the following steps: dispersing Envidor evenly and carrying out continuous sanding to obtain a suspending agent, then using the aqueous solution of the emulsifier and the adhesive to prepare emulsion, and mixing the suspending agent with the emulsion evenly to obtain the suspoemulsion (SE) containing Envidor. Envidor is used as a new bactericide to prepare a new environmentally friendly pesticide preparation, namely SE; and the dosage of the organic solvent used in the traditional emulsifiable concentrate preparation is reduced, environmental pollution can be reduced and the toxicity to the user can be reduced. The SE has stable performance, the layering and precipitation can be avoided, crystal growth can not be prevented, and SE is convenient to use.
Description
Technical field
The present invention relates to formulations of pesticide manufacture field, be specifically related to tetronic acid class miticide spiral shell mite ester and prepare the suspension system of former medicine particulate and oil-like emulsions component and be mixed and form stable suspended emulsion, with and preparation method thereof.
Background technology
Spiral shell mite ester physicochemical property: appearance white powdery, without special odor, fusing point: 94.8 ℃, 20 ℃, vapour pressure 3 * 10
-7pa, 20 ℃ of density 1.29g/cm
3.Dissolubility (material/1000ml solvent, 20 ℃): in n-hexane 20, in carrene, > 250, in isopropyl alcohol 47, in dimethylbenzene, > 250, in water 0.05.Toxicity: rat acute LD50 of passing through mouth > 2500mg/kg, acute through skin LD50 > 4000mg/kg; To a honeybee LD50 > 100 μ g/ honeybee.The mode of action: have the brand-new mechanism of action, tool action of contace poison, does not have interior absorption.The main Fatty synthesis that suppresses mite, the energy metabolism of blocking-up mite, each developmental stage of mite is all effective, comprises ovum.Spiral shell mite ester belongs to novel tetronic acid class miticide, it does harm to the Fatty synthesis in mite body by inhibition, destroy the energy metabolism activity of acarid, finally kill harmful mite, be a kind of new, efficient non-internal-absorting leaf surface treatment miticide, do not have cross resistance problem with other existing miticide, the different mite classes of various crop are all had to fine preventive effect and outstanding lasting effect, not only ovicidal but also kill young mite, was particularly suitable for control and existing miticide was produced to the pest mite class of resistance.
Suspension emulsion suspoemulsion, is abbreviated as SE, is the higher suspension emulsus system of disperseing homogenizing to form in aqueous medium by the former medicine of a kind of water-fast solid and a kind of oily liquids and various auxiliary agent.Be three mixtures, organic facies (discontinuous phase) is scattered in water (continuous phase), i.e. oil/water type emulsion and the solid that is dispersed in water completely.It has advantages of suspending agent and aqueous emulsion, as has avoided emulsifiable concentrates for agricultural chemicals and wetting powder because organic solvent and dust are to environment and operator's pollution and murder by poisoning, and storing safety, has higher biologically active etc.
Summary of the invention
Therefore, the spiral shell mite ester suspension emulsion that provides a kind of stable in properties, crystal not to grow up is provided the technical problem to be solved in the present invention.
Another technical problem that the present invention will solve is to provide the preparation method of this spiral shell mite ester suspension emulsion.
Technical scheme of the present invention is, a kind of suspension emulsion containing spiral shell mite ester, described suspension emulsion comprises: spiral shell mite ester 1～50 weight portion, wetting dispersing agent 2～10 weight portions, antigraining agent 1～3 weight portion, defoamer 0.1～2 weight portion, sticker 1～25 weight portion, emulsifier 2～10 weight portions, water 0.1-100 weight portion.
According to the suspension emulsion containing spiral shell mite ester of the present invention, preferably, described suspension emulsion also can comprise antifreeze 0.1～10 weight portion, thickener 0.005-2 weight portion, preservative 0.005-2 weight portion.
In a preferred embodiment, described wetting dispersing agent is selected from: macromolecule EO-PO block copolymer, naphthalenesulfonic acid-formaldehyde condensate, fatty alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, macromolecule is dredged a dress copolymer of type, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styryl phenol polyethenoxy polyethenoxy ether, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, alkyl naphthalene formaldehyde condensate sulfonates, lignosulfonates, one or more kinds of combinations in polymerization of carboxylic acid salt.More preferably, described wetting dispersing agent is selected from a kind of or its mixing in Pluronic PE 6800 or alkylphenol-polyethenoxy formaldehyde condensation products sulphate.
In a preferred embodiment, described emulsifier is selected from this dish SPAN series, soil temperature TWEEN series, NP series Nonyl pheno, polyoxyethylene nonylphenol ether phosphate, AEO series fatty alcohol-polyoxyethylene ether, macromolecule EO-PO block copolymer, alkylphenol-polyethenoxy polyethers and sulphate thereof, alkylphenol-polyethenoxy polyethers phosphoric acid fat, alkylphenol polyoxyethylene formaldehyde condensation products sulphate phosphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, one or more kinds of combinations in styryl phenol polyethenoxy polyethenoxy ether.
In a preferred embodiment, described antigraining agent is water miscible large molecule or inorganic salts compound.
Further, described antigraining agent is selected from: the one or more kinds of combinations in PVAC polyvinylalcohol, polyvinylpyrrolidone PVP, polyethylene glycol PEG, Sodium Polyacrylate PAAS, urea, sodium chloride, potassium chloride, magnesium sulfate, sodium sulphate, potassium nitrate.More preferably, antigraining agent is a kind of or its combination in polyvinylpyrrolidone PVP, polyethylene glycol PEG.
In a preferred embodiment, described sticker is selected from: the one or more kinds of combinations in vegetable oil and derivative thereof, mineral oil, atoleine (being white oil), fatty acid mixt, long-chain oleic acid, linear paraffin solvent naphtha, cycloalkane solvent naphtha.
Described vegetable oil is soybean oil, rapeseed oil, cottonseed oil, Semen Ricini oil, palm oil, corn oil, turpentine oil, cocoa butter, sunflower oil, loose base oil etc. preferably.The derivative of vegetable oil can be methylated vegetable oil, epoxidized vegetable oil, tree tar etc.More preferably, sticker is a kind of or its mixture in vegetable oil and methylated vegetable oil.
Preferably, described defoamer is selected from a kind of in silicon defoamer, polyethers defoamer, higher alcohols, tributyl phosphate, polysiloxane defoamers.
The water adopting in this production technology is deionized water or distilled water.
Preferably, described antifreeze is a kind of in ethylene glycol, propane diols, glycerine, isopropyl alcohol, urea, sodium chloride.
Preferably, described thickener is selected from: the one or more kinds of combinations in xanthans, cellulose ether and derivative thereof, polyvinyl alcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, white carbon, gelatin, gum Arabic.
Preferably, described preservative is: a kind of in the methylol organic matter of formaldehyde, glutaraldehyde, potassium sorbate, Sodium Benzoate, polycondensation, isothiazolinone.Thickener and preservative can add as required in right amount.The methylol organic matter of polycondensation is release formaldehyde type.
The present invention also provides the above-mentioned preparation method containing spiral shell mite ester suspension emulsion, and the method comprises the following steps:
(1) water is mixed with wetting dispersing agent, antigraining agent, defoamer, after the former medicine of input spiral shell mite ester is uniformly dispersed, by sand mill, carry out serialization sand milling, obtain the suspending agent SC of spiral shell mite ester;
(2) by emulsifiers dissolve in sticker, after mixing, obtain oil phase, emulsifier and water are mixed and made into water, the oil phase configuring is poured into water and is opened high speed homogenizing, form stable O/W emulsion;
(3) emulsion that adds step (2) to obtain in the spiral shell mite ester suspending agent SC preparing, mixes, and obtains spiral shell mite ester suspension emulsion SE.
Preferably, described sand milling temperature is 0-40 ℃; Spiral shell mite ester particle diameter after described sand milling is 1 μ m-8 μ m.
Further, in described step (3), also can add antifreeze 0.1～10 weight portion, thickener 0.005-2 weight portion, preservative 0.005-2 weight portion.
In preparation method, the preferable range of various components is the same.
Spiral shell mite ester is prepared into environment-friendly pesticide novel form suspension emulsion SE as a kind of new type bactericide, reduces the organic solvent that traditional cream preparation is used, and can reduce environmental pollution, reduces the toxicity to operator.Spiral shell mite ester is a kind of efficient non-internal-absorting leaf surface treatment miticide, tool action of contace poison, and there is no interior absorption, by formulation optimization, intend finding a kind of method of active ingredient spiral shell mite ester to the efficiency of tagging of target insect that improve in the present invention.
In suspension emulsion of the present invention, oil component exists in whole suspension system with the form of emulsion particle, and under the former medicine normal temperature of spiral shell mite ester, be lenticular, one height degree of sticking together oil component (sticker) of the present invention's screening, improve the adhesive force of active ingredient spiral shell mite ester particulate to target crop and insect, prepared stable emulsion system simultaneously.And this height degree of sticking together oil component (sticker) should be water insoluble or has micro-solvability in water.The spiral shell mite ester suspension emulsion making should be stable at the temperature of production and product duration of storage, can not have crystallization.
Suspension emulsion is that disperse phase (comprising: solia particle and emulsion particle) stable and uniform is dispersed in and take among the medium that water is continuous phase, because emulsion dispersion belongs to unsettled system on thermodynamics, easily cause coacervation or emulsion attached collection breakdown of emulsion in solid dispersed phase of system.So the emulsifier of the present invention's screening can effectively be avoided this point, obtains stable suspension emulsion.In suspension emulsion, one or more components are that the form of emulsion particle is distributed in whole system, can use the former medicine of some dissolution with solvents solids or dilute the former medicine of full-bodied liquid.Can cause suspension emulsion under these solvent actions in, there is the phenomenon that oiling dissolves on the part solia particle surface of solid dispersed phase, and causes and the problem of Ostwald ripening (generate crystallization and crystal is grown up) finally cause the unstable of suspension emulsion.The present invention effectively avoids the appearance of above-mentioned phenomenon by screening suitable wetting dispersing agent.And common spiral shell mite ester suspending agent product still has the unsettled situation of suspension system, solia particle easily occurs that crystal is grown up and the phenomenon of formula slaking difficult to understand, the present invention has searched out a kind of antigraining agent, for preventing that the particle of suspension system from increasing, thereby forms stable suspension system.
The invention has the beneficial effects as follows:
1, in suspension system, add height degree of sticking together oil-like emulsions component (sticker) the formation suspension emulsion that is mixed, make brute force adhesion and the crop surface of solia particle after foliage spray, improve resistance to rainwash ability; And strengthened the cohesive force of the body surface that is attached to mite pest, improve the effect of tagging.Extend the holdup time of active ingredient spiral shell mite ester on crop simultaneously, thus significantly synergy.
2, selected oil component derives from plant resource or mineral oil, and without poisoning, security performance is high; Take water as continuous media, can effectively reduce to the excitant of skin and eyes and toxicity safety, environmental protection; With an organic solvent the usage amount of (as: toluene, xylene), does not avoid inflammable, explosive and poisoning problem in production; Packing, storage and freight reduce, and save production cost.
3, in suspension emulsion of the present invention, the former medicine of spiral shell mite ester exists in whole suspension system with the form of solia particle, this former medicine belongs to the former medicine of medium fusing point (94.8 ℃ of fusing points), the general method of pulverizing has dry pulverization process and wet pulverizing, the broken way of the former medicinal powder of solid in the present invention, selects the former medicine of wet method hypothermia grait abrasive dust broken spiral shell mite ester.It is in stable condition that low temperature wet pulverizing has the broken former medicine of physics, and final formulation products is difficult for livering; Can serialization produce, production efficiency is higher; During production, working environment is to human body safety, there is no the pollution factors such as noise in dry pulverization process, dust, waste gas.
4, preparation method's cost of the present invention is low, is convenient to suitability for industrialized production.
Embodiment
In order better to illustrate, can further illustrate the technology of the present invention by following instantiation, but tightly not be limited to this.
Embodiment mono-
The first step: by 150g deionized water and Morwet EFW 10g (wetting agent of Akzo Nobel N.V.'s Negel), Morwet D-425 20g (Akzo Nobel N.V.'s alkyl naphthalene sulfonic acid condensation polymer sodium salt dispersant), antigraining agent PVAC polyvinylalcohol 5g, silicone defoaming agent 5g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 50g is uniformly dispersed, by horizontal sand mill, carry out serialization sand milling, sand milling temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 3 μ m ± 2 μ m) after reaching claimed range, obtain the suspending agent SC of spiral shell mite ester.
Second step: Alkamus VO/01 20g (Rhodia's emulsifier) is dissolved in the corn oil of 200g (commercial material), obtains oil phase after stirring; To in the deionization of the AEO-12 of 30g (Hai'an petro-chemical corporation fatty alcohol-polyoxyethylene ether emulsifier production), 309g, stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable O/W emulsion, obtain sticker corn oil emulsion.
The 3rd step: add the sticker corn oil emulsion 559g preparing in the spiral shell mite ester suspending agent SC 240g preparing, open simultaneously and stir (maintaining 300 turn/min), then xanthans (2%) aqueous solution, bactericide MTI 1g (2-methyl-4 that add ethylene glycol 100g, 100g, isothiazolinone compounds), stir 5-propylidene-4-isothiazoline-3-ketone:, make 5% spiral shell mite ester suspension emulsion SE.
Embodiment mono-, the key technical indexes are as following table:
Embodiment bis-:
The first step: by 150g deionized water and Igepal BC/100 10g (Rhodia's polyethenoxy ether class wetting agent), TRITON XN-45S 30g (Dow Chemical's sulfuric acid ester dispersant), antigraining agent (PVP) K-30 10g, silicone defoaming agent 5g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 100g is uniformly dispersed, by vertical grinding machine, carry out sand milling, grinding temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 3 μ m ± 2 μ m) after reaching claimed range, obtains the suspending agent SC of spiral shell mite ester.
Second step: Atplus 300F 20g (standing grain major company mineral oil emulsifier) is dissolved in to (commercial material) in 200g mineral oil and obtains oil phase after stirring; To in the deionization of the Soprophor 3D33 of 30g (Rhodia's emulsifier production), 250g, stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable O/W emulsion, obtain sticker mineral oil emulsion.
The 3rd step: add the sticker mineral oil emulsion 500g preparing in the spiral shell mite ester suspending agent SC 305g preparing, open simultaneously and stir (maintaining 300 turn/min), then add propane diols 50g, bactericide BIT 1g (1, isothiazolinone compounds), sodium carboxymethylcellulose CMC 10g, deionized water supply 1000g and stir, and makes 10% spiral shell mite ester suspension emulsion SE 2-benzisothiazole-3-ketone:.
Embodiment bis-, the key technical indexes are as following table:
Embodiment tri-:
The first step: by 250g deionized water and ECOSURF EH-9 10g (Dow Chemical's polyethenoxy ether class wetting agent), Sorphophor FD 40g (Rhodia's phosphoric acid ester dispersant), antigraining agent Sodium Polyacrylate PAAS 5g, polyethers defoamer 10g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 250g is uniformly dispersed, by horizontal sand mill, carry out serialization sand milling, grinding temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 3 μ m ± 2 μ m) after reaching claimed range, obtains the suspending agent SC of spiral shell mite ester.
Second step: Emulsogen EL 20g (Clariant company emulsifier production) is dissolved in to (Exxon Mobil Corporation's solvent naphtha) in ISOPAR M 200g solvent naphtha and obtains oil phase after stirring; The Ethylan 500QL of 40g (Aksu company emulsifier production) joined in the 575g spiral shell mite ester suspending agent SC preparing, add again in the deionization of 94g and stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspended emulsion.
The 3rd step: open and stir (maintaining 200 turn/min), then add white carbon (8%) aqueous solution, the bactericide Sodium Benzoate 1g (commercial) of antifreeze urea 30g, thickener 50g to stir, make 25% spiral shell mite ester suspension emulsion SE.
Embodiment tri-, the key technical indexes are as following table:
Embodiment tetra-
The first step: by 350g deionized water and Morwet EFW 10g (the naphthalenesulfonic acid-formaldehyde condensate wetting agent of Akzo Nobel N.V.), MorwetD-425 40g (the Fluhyzon formaldehyde condensation products Sulfonates dispersant of Akzo Nobel N.V.), antigraining agent (PVP) K-90 10g, polyethers defoamer 10g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 300g is uniformly dispersed, by horizontal sand mill, carry out serialization sand milling, grinding temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 5 μ m ± 3 μ m) after reaching claimed range, obtain the suspending agent SC of spiral shell mite ester.
Second step: PE-6100 20g (EO/PO of BASF AG block emulsifier production) is dissolved in to (commercial) in loose base vegetable oil 150g solvent naphtha and obtains oil phase after stirring; The PE-10500 of 40g (EO/PO of BASF AG block emulsifier production) joined in the 720g spiral shell mite ester suspending agent SC preparing, add again in the deionization of 8g and stir evenly (water); The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspended emulsion.
The 3rd step: open and stir (maintaining 200 turn/min), then add antifreeze ethylene glycol 50g, thickener hydroxyethylcellulose HEC 10g, bactericide glutaraldehyde 2g (commercial) to stir, make 30% spiral shell mite ester suspension emulsion SE.
Embodiment tetra-, the key technical indexes are as following table:
Embodiment five
The first step: by 350g deionized water and ECOSURF EH-6 10g (Dow Chemical's polyethenoxy ether class wetting agent), TERGITOL XJ 40g (EO-PO of Dow Chemical copolymer dispersant), antigraining agent PEG-400 10g, tributyl phosphate 5g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 400g is uniformly dispersed, by vertical little sand mill (2L), carry out clearance-type sand milling, grinding temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 5 μ m ± 3 μ m) after reaching claimed range, obtains the suspending agent SC of spiral shell mite ester.
Second step: Geronol VO/02N 20g (Rhodia's emulsifier production) is dissolved in to (Yueyang petrochemical industry) in 100g paraffin oil and obtains oil phase after stirring; The AG530 of 20g (Aksu company emulsifier production) is joined in the 865g spiral shell mite ester suspending agent SC preparing and stirs evenly and obtain water; The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspended emulsion.
The 3rd step: open and stir (maintaining 200 turn/min), then aluminium-magnesium silicate (8%) aqueous solution, the bactericide KF88 1g (commercial) that add antifreeze urea 30g, thickener 30g, moisturizing quantitatively stirs to 1000g, makes 40% spiral shell mite ester suspension emulsion SE.
Embodiment five the key technical indexes are as following table:
Embodiment six
The first step: by 300g deionized water and TERSPERSE 4896 10g (Hensel Man wetting agent), TERGITOL XD 40g (EO-PO of Dow Chemical copolymer dispersant), antifreeze propane diols 30g, antigraining agent k-30 (PVP) 10g, silicone defoaming agent 10g mixing and stirring, then after the former medicine of spiral shell mite ester that drops into 500g is uniformly dispersed, by horizontal little sand mill, carry out serialization sand milling, grinding temperature is controlled at below 40 ℃, granularity stops sand milling (average grain diameter 5 μ m ± 3 μ m) after reaching claimed range, obtains the suspending agent SC of spiral shell mite ester.
Second step: Atlox 4838B 10g (Clariant company emulsifier production) is dissolved in to (commercial) in 50g esterification soybean oil and obtains oil phase after stirring; The Genapol O-100 of 10g (standing grain major company emulsifier production) is joined in the 900g spiral shell mite ester suspending agent SC preparing and stirs evenly and obtain water; The oil phase configuring, to entering water and opening high speed homogenizing, is formed to stable suspended emulsion.
The 3rd step: open to stir (maintaining 200 turn/min), then add, xanthans (2%) aqueous solution of thickener 29g, bactericide formaldehyde 1g (commercial) stirs, and makes 50% spiral shell mite ester suspension emulsion SE.
Embodiment six the key technical indexes are as following table:
Embodiment test of pesticide effectiveness result: our considering cost, use the factors such as consumption, dispenser custom, adopt content 25% spiral shell mite ester SE suspension emulsion more reasonable as test medicine.
1 materials and methods
1.1 test sites and condition
Common orchard, managerial skills are medium, and experimental cultivar is Red Star, seeding row spacing 3m * 4m, fruit tree growth is basically identical, 2000 kilograms of left and right of per mu yield, the generation over the years of this garden European red mite is heavier.
1.2 experimental scheme and method
5 processing are established in test altogether: 25% spiral shell mite ester suspension emulsion SE4000,5000,6000 times of liquid, contrast medicament is respectively SC4000 times of liquid of 25% spiral shell mite ester suspending agent, 50% spirodiclofen water dispersible granule WDG8000 times liquid, contrast spray clear water.Every 2 strain trees are 1 community, and randomized arrangement, repeats 4 times.Formulation rate take blade even medicine, slightly medicine drip drop down as degree, every liquid 4 for strain.
1.3 investigation statistics methods
2 strain test trees are all investigated in every community.Every tree by east, south, west, north, in 5 orientation, every orientation is chosen 5 leafage branch listing marks that blade is intact at random, 1 mite mouth radix of investigation before medicine.Within after dispenser medicine 1,7,28 day, respectively investigate mite number alive 1 time; The significance level of difference by " DMRT " method check drug effect.
2 results and analysis
First group of 25% spiral shell mite ester suspension emulsion SE and 25% spiral shell mite ester suspending agent SC results of comparison: investigation in 7 days after medicine, the preventive effect of 25% 4000,5000,6000 times of liquid of spiral shell mite ester suspension emulsion SE and 4000 times of liquid of contrast medicament 25% spiral shell mite ester suspending agent SC reaches respectively 98.78%, 99.32%, 96.45%, 87.15%.Test of significance shows. the preventive effect of 3 concentration of spiral shell mite ester suspension emulsion SE is all significantly higher than contrast medicament spiral shell mite ester suspending agent SC; Investigation in 28 days after medicine, the preventive effect of 25% spiral shell mite ester suspension emulsion SE4000,5000,6000 times of liquid and 4000 times of liquid of contrast medicament 25% spiral shell mite ester suspending agent SC is respectively 95.84%, 92.82%, 97.62% and 80.32%.The preventive effect of the spiral shell mite ester suspension emulsion SE of 3 concentration is all significantly higher than contrast medicament spiral shell mite ester suspending agent SC, and the preventive effect difference between 3 concentration processing is not remarkable.The survey showed that, and the relative suspending agent SC lasting period of spiral shell mite ester suspension emulsion SE is long.
Second group of 25% spiral shell mite ester suspension emulsion SE and 50% spirodiclofen water dispersible granule WDG results of comparison: investigation in 1 day after medicine, the preventive effect of 25% 4000,5000,6000 times of liquid of spiral shell mite ester suspension emulsion SE and contrast medicament 50% spirodiclofen water dispersible granule WDG8000 times liquid is respectively 84.37%, 83.17%, 86.51% and 78.32%.Test of significance, the preventive effect that each concentration of 25% spiral shell mite ester suspension emulsion SE is processed is significantly higher than 8000 times of liquid of 50% spirodiclofen water dispersible granule WDG, and quick-acting is better than WDG; After medicine 7 days, the preventive effect of 25% spiral shell mite ester suspension emulsion SE significantly improved, and 4000, the preventive effect of 5000,6000 times of liquid and 8000 times of liquid of contrast medicament 50% spirodiclofen water dispersible granule WDG is respectively 99.24%, 99.49%, 98.63% and 92.32%.Test of significance, all there were significant differences with contrasting medicament for the preventive effect of 3 concentration of 25% spiral shell mite ester suspension emulsion SE; Investigation in 28 days after medicine, the preventive effect of 25% 4000,5000,6000 times of liquid of spiral shell mite ester suspension emulsion SE and 8000 times of liquid of contrast medicament 50% spirodiclofen water dispersible granule WDG is respectively 95.37%, 92.16%, 91.73%, 85.73%.Test of significance, the preventive effect of 3 concentration of 25% spiral shell mite ester suspension emulsion SE is all significantly higher than 8000 times of liquid of contrast medicament 50% spirodiclofen water dispersible granule WDG.Visible reagent agent spiral shell mite ester suspension emulsion SE has the longer lasting period than contrast medicament spirodiclofen water dispersible granule WDG.
Duration of test, does not find that reagent agent has harmful effect to growth and development of fruit tree, fruit appearance and output; Safer to predators such as Chrysopa, ladybug, minute pirate bugs.
3 interpretations of result and discussion
Result of the test shows, 25% spiral shell mite ester suspension emulsion SE is good to apple tree two spotted spider mite preventive effect; Control apple tree two spotted spider mite drug action speed will be faster than spiral shell mite ester suspending agent SC and spirodiclofen water dispersible granule WDG, and dispenser reached favorable effect after 3 days; Lasting period extends than spiral shell mite ester suspending agent SC and spirodiclofen water dispersible granule WDG; The preventive effect difference of 3 concentration is not obvious; To apple tree safety.
Claims (7)
1. the suspension emulsion containing spiral shell mite ester, it is characterized in that: described suspension emulsion comprises: spiral shell mite ester 1～50 weight portion, wetting dispersing agent 2～10 weight portions, antigraining agent 1～3 weight portion, defoamer 0.1～2 weight portion, sticker 1～25 weight portion, emulsifier 2～10 weight portions, water 0.1-100 weight portion; Described antigraining agent is selected from: the one or more kinds of combinations in PVAC polyvinylalcohol, polyvinylpyrrolidone PVP, polyethylene glycol PEG, Sodium Polyacrylate PAAS;
Described sticker is selected from: the one or more kinds of combinations in vegetable oil and derivative thereof, mineral oil, atoleine, fatty acid mixt, long-chain oleic acid, linear paraffin solvent naphtha, cycloalkane solvent naphtha;
Described wetting dispersing agent is selected from: macromolecule EO-PO block copolymer, naphthalenesulfonic acid-formaldehyde condensate, fatty alcohol polyethenoxy ether class, alkylphenol polyoxyethylene class, alkylphenol-polyethenoxy formaldehyde condensation products sulphate, the dendritic copolymer of macromolecule comb type, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, styryl phenol polyethenoxy polyethenoxy ether, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, alkyl naphthalene formaldehyde condensate sulfonates, lignosulfonates, one or more kinds of combinations in polymerization of carboxylic acid salt,
Described emulsifier is selected from the one or more kinds of combinations in this dish SPAN series, soil temperature TWEEN series, the serial fatty alcohol-polyoxyethylene ether of AEO, macromolecule EO-PO block copolymer, alkylphenol-polyethenoxy polyethers and sulphate thereof, alkylphenol-polyethenoxy polyethers phosphoric acid fat, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether.
2. the suspension emulsion containing spiral shell mite ester according to claim 1, is characterized in that: described suspension emulsion also comprises antifreeze 0.1～10 weight portion thickener 0.005-2 weight portion, preservative 0.005-2 weight portion.
3. the suspension emulsion containing spiral shell mite ester according to claim 1, is characterized in that:
Described defoamer is selected from a kind of in silicon defoamer, polyethers defoamer, higher alcohols, tributyl phosphate, polysiloxane defoamers.
4. the suspension emulsion containing spiral shell mite ester according to claim 2, is characterized in that:
Described antifreeze is a kind of in ethylene glycol, propane diols, glycerine, isopropyl alcohol, urea, sodium chloride;
Described thickener is selected from: the one or more kinds of combinations in xanthans, cellulose ether and derivative thereof, polyvinyl alcohol, aluminium-magnesium silicate, bentonite, kaolin, diatomite, white carbon, gelatin, gum Arabic;
Described preservative is: a kind of in the methylol organic matter of formaldehyde, glutaraldehyde, potassium sorbate, Sodium Benzoate, polycondensation, isothiazolinone.
5. described in claim 1-4 any one, contain the preparation method of the suspension emulsion of spiral shell mite ester, it is characterized in that: the method comprises the following steps:
(1) water is mixed with wetting dispersing agent, antigraining agent, defoamer, after the former medicine of input spiral shell mite ester is uniformly dispersed, by sand mill, carry out serialization sand milling, obtain the suspending agent SC of spiral shell mite ester; Described sand milling temperature is 0-40 ℃;
(2) by emulsifiers dissolve in sticker, after mixing, obtain oil phase, emulsifier and water are mixed and made into water, the oil phase preparing is poured into water and is opened high speed homogenizing, form stable O/W emulsion;
(3) emulsion that adds step (2) to obtain in the spiral shell mite ester suspending agent SC preparing, mixes, and obtains spiral shell mite ester suspension emulsion SE claimed in claim 1.
6. the preparation method containing spiral shell mite ester suspension emulsion according to claim 5, is characterized in that: the spiral shell mite ester particle diameter after described sand milling is 1 μ m-8 μ m.
7. the preparation method containing spiral shell mite ester suspension emulsion according to claim 5, is characterized in that: in described step (3), also add antifreeze 0.1～10 weight portion, thickener 0.005-2 weight portion, preservative 0.005-2 weight portion.
Priority Applications (1)
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| CN102696655B (en) * | 2012-05-24 | 2013-11-27 | 永农生物科学有限公司 | Compound pesticide composition containing spirodiclofen and preparation thereof |
| CN106818883A (en) * | 2016-12-15 | 2017-06-13 | 东莞市联洲知识产权运营管理有限公司 | The compounding suspension emulsion and preparation method of a kind of herbicide and plant growth regulator |
| CN107494561A (en) * | 2017-10-03 | 2017-12-22 | 江苏长青生物科技有限公司 | A kind of tricyclazole aqueous suspension agent composition |
| CN109757473B (en) * | 2019-02-25 | 2021-12-28 | 上海生农生化制品股份有限公司 | Crystallization inhibition composition, application and crystallization inhibition method |
| CN110150283B (en) * | 2019-05-27 | 2021-04-16 | 中农立华生物科技股份有限公司 | Spirodiclofen suspending agent and preparation method thereof |
| CN113875763B (en) * | 2021-10-29 | 2022-07-22 | 黑龙江省农业科学院植物保护研究所 | Chelerythrine suspending agent and preparation method and application thereof |
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| CN102228027A (en) * | 2011-05-06 | 2011-11-02 | 陕西韦尔奇作物保护有限公司 | Pesticide composition containing fenazaquin |
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