CN104686542A - Fluacrypyrim composition containing ultralow-capacity liquid and preparation method thereof - Google Patents
Fluacrypyrim composition containing ultralow-capacity liquid and preparation method thereof Download PDFInfo
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Abstract
The invention discloses fluacrypyrim composition containing ultralow-capacity liquid and a preparation method thereof, and belongs to the field of pesticides. The composition comprises the following components in percentage by weight: 1 to 50% of active ingredient, 5 to 30% of surface active agent, and the balance of carrier, wherein the active ingredient includes fluacrypyrim and bifenazate in weight ratio of 1: 3. The fluacrypyrim composition containing ultralow-capacity liquid is safe, environmentally friendly, stable to store, and good in acaricidal effect and can be used for preventing pest mites of fruit trees. The invention further provides the preparation method of the fluacrypyrim composition containing ultralow-capacity liquid.
Description
Technical field
The invention belongs to pesticide field, be specifically related to a kind of ultra low volume liquids containing fluacrypyrim composition and preparation method thereof.
Background technology
Day by day dense and under the demand situation of pollution-free food to environmental protection consciousness current people; it is also more and more stricter that relevant laws and regulations are made in the safety of many countries to agricultural chemicals; in order to meet the object of agricultural production needs and protection of the environment; agricultural chemicals workers, while the research and development of reinforcement pesticide new variety, focus on the research to the formulations of pesticide more.
Because conventional spray-on process makes the formulation of with medicament be generally missible oil, aqua, wetting powder, suspending agent, aqueous emulsion etc., certain defect is there is: when 1) using, need large water gaging on using, usual water consumption reaches 450-900L/ha, liquid is after large water gaging dilution, surface tension is often larger, adhesiveness on the crop having wax coat or target surface, wetability, permeability are poor, are difficult to effectively enter in crop and target body, cause preventive effect poor; 2) in illumination, high temperature, dry natural environment, the water in liquid is easy to evaporation, causes medicament only to remain in crop surface, easy photodissociation and drying easy coming off from crop and losing efficacy afterwards; 3) mist droplet particle size of conventional spraying is comparatively large, reaches 200-600 μm, causes the liquid be sprayed onto on crop or target surface easily to run off; 4) conventional spray-on process work efficiency is low.5) a lot of away from water source and drought and water-scarce area, conventional spray-on process is difficult to carry out or can not reaches desirable control efficiency.Along with the enforcement of China's land transformation policy, soil presents the trend of intensive management, there is increasing agricultural planting rich and influential family, crop contiguous plant area increases, in addition, along with the appearance of China's aging population and recruitment famine, labour becomes rare resource just gradually, human cost improves constantly, and agriculture production cost continues to increase; Agricultural production is obviously seasonal, and damage by disease and insect often needs a large amount of manpower to prevent and treat at short notice, adopts the application technique of existing dosage form product, is difficult to the needs meeting large-scale planting.
Ultra low volume spraying is appearance with ultra low volume sprayer tool and the advanced applications of pesticide new technology of of producing.The solvent that ultra low volume liquids is low by screening volatility, flash-point is high, good, low to chemical injury of crops to former medicine dissolubility, viscosity is low, be not watered during dispenser, but directly use with ultra low volume sprayer tool, low-gallonage spraying apparatus or ultra low volume electrostatic spray apparatus.Ultra low volume spraying due in droplet not containing high volatile ingredient, its size and quality arrive target process do not have significant change from leaving apparatus of spray, decrease to volatilize and elegant.Droplet is tiny and even, meets " biological best granula " requirement, significantly improves deposition.Owing to using without the need to being watered, ultra low volume liquids is suitable for water scarcity, damage by disease and insect fulminant large area occurs and the occasion of dispenser on a large scale in the palpus short time, and ultra low volume spraying simultaneously reduces the labour intensity of operator greatly.
Fluacrypyrim (chemical name: (E)-2-α-[2-isopropoxy-6-(trifluoromethyl) pyrimidine-4-yl oxygen base]-o-tolyl)-3-methoxy-methyl acrylate) be first the methoxy acrylic miticide developed by BASF AG's development, Japanese Cao Da company.Be mainly used in control fruit tree if the multiple mite class in apple, citrus, pears etc. is as European red mite, citrus red mite etc.
Bifenazate (chemical name: isopropyl 3-(4-methoxyl biphenyl base-3-base) carbazates) equals report in 1996 by M.A.Dekeyser, found by Uniroyal company and developed jointly, in biphenyl hydrazine class, non-internal-absorting, the new selective foliar spray miticide of listing in 2000 by Uniroyal company and Nissan company.Food leaf class acarid in main control oranges and tangerines, grape, fruit tree, vegetables, cotton, corn and ornamental plants, as each stage of Panonychus citri, T.urticae Koch, especially has ovicidal action to Tetranychus urticae.Effective to each developmental stage of mite, there is ovicidal activity and knock down activity (48 ~ 72h) with to what become mite.Minimum on predacious mite impact, be very suitable for the comprehensive regulation of insect.Do not have poison to plant, the lasting period is long.
Although this miticide composition can be mixed with water dispersible granules, suspending agent, wetting powder, missible oil or aqueous emulsion agent, for preventing and treating the mite class on citrus red mite, European red mite, cotton crop.But in recent years, along with improving constantly of human living standard, the health problem of food and environment receives the concern of people day by day, thus countries in the world all increase the exploitation dynamics to novel pesticide and novel form.Ultra low volume liquids is a kind of high-efficiency low-toxicity, the agricultural chemicals novel formulation of low-residual, it be a kind of with the oily solvent of high-flash for pesticide activity component dispersion medium, add the special finish of one that suitable cosolvent and auxiliary agent are mixed with.This formulation adhesiveness on crop or target surface is good, wetability, permeability are strong, thus, not only biologically active is good, and quick-acting is high, lasting effect is long, good to crop safety, and environmentally friendly, to non-target safety such as people and animals, dispenser water consumption can be saved, meet the security requirement of pesticidal preparations, meet the various requirement of agricultural sustainable development.There is not been reported both at home and abroad for fluacrypyrim and the composite ultra low volume liquids of Bifenazate.
Summary of the invention
The invention provides the ultra low volume liquids and preparation method thereof containing fluacrypyrim composition, the present invention overcomes the defects such as the work efficiency that conventional control fruit tree evil mite method exists is low, labour intensity large, liquid dilution needs many, the anti-heterodynes of water, the lasting period is short, resistance.Inventor of the present invention is devoted to the research of the ultra low volume liquids novel form containing fluacrypyrim composition, its object is to: on the one hand, there is provided a kind of safety, environmental protection, stable storage, miticidal effect good containing the ultra low volume liquids preparation of fluacrypyrim with Bifenazate, do harm to mite for preventing and treating fruit tree.On the other hand, a kind of preparation method of the ultra low volume liquids containing fluacrypyrim composition is provided.
For solving the problem, the present invention adopts following technical scheme: containing the ultra low volume liquids of fluacrypyrim composition, said composition forms by by active component, surfactant and carrier, and the weight percentage of each component is: active component 1 ~ 50%, surfactant 5 ~ 30%, surplus are carrier; Wherein, active component is fluacrypyrim, Bifenazate, and the two relative scale is 1: 3 based on the number of active component weight.Preferably: in composition, the weight percentage of active component is 10% ~ 30% of gross weight.
Described surfactant is following one or at least two kinds of mixtures: ethoxylated castor oil, polyoxyethylene (n20) phenethyl phenol ether through reaction oleate, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate, alkylaryl formaldehyde resin APEO, triphenyl vinyl phenol polyoxyethylene (n
20) ether phosphoric acid triethanolamine salt, castor oil polyoxyethylene ether, Ben-zylphenol Polyoxyethyl Ether, diphenyl phenolic group polyoxyethylene (n
18) ether formaldehyde condensation products, agriculture breast Atlox 4838B, agriculture breast Atlox 4914, agriculture breast Atsurf 3300B, agriculture breast Atlas G5000, agriculture breast LEW-O, agriculture breast LME-2, agriculture breast LME-4, agriculture breast LME-5, agriculture breast LEW-5, agriculture breast LEW-50, agriculture breast PICO-LE25, agriculture breast AEO-3, agriculture breast 0201B, agriculture breast 0203B, agriculture breast T-20, agriculture breast T-80, agriculture breast T-85, agriculture breast S-80, agriculture breast 507#, agriculture breast 100#, agriculture breast 36#, agriculture breast 500#, agriculture breast 600#, Nongru-700 #, agriculture breast 1601#, agriculture breast OX-2681, agriculture breast 2201#, agriculture breast NP-7, agriculture breast NP-10, agriculture breast NP-15, agriculture breast OX-635, agriculture breast OX-653, agriculture breast OX-690, agriculture breast OX-8686, agriculture breast PICO-LOE, agriculture breast P work CO-LE1.
Described carrier is following one or at least two kinds of mixtures: diethyl malonate, pimelic acid diethylester, diethyl maleate, triacetyl glycerine, tetraethyleneglycol dimethyl ether, butyl cellosolve, diethylene glycol acetate, diethylene glycol monoethyl ether, diethylene glycol diethyl ether, diethylene glycol monobutyl ether, diethyl oxalate, ethylene sebacate, solvent naphtha 150#, solvent naphtha 180#, solvent naphtha 200#, solvent naphtha D80, repefral, dibutyl phthalate, dioctyl phthalate, o-dichlorohenzene, acetophenone, cyclohexanone, 1-METHYLPYRROLIDONE, N, dinethylformamide, N, N-dimethylacetylamide, phenmethylol, methyl-sulfoxide, diethylene glycol acetate, n-hexyl alcohol, n-octyl alcohol, Liquid Macrogol, PEG400, methyl oleate, ethyl oleate, olein, glycerin monostearate, castor oil methyl esters, triethylene Glycol ether, epoxidized soybean oil, cottonseed oil, rapeseed oil, corn oil, castor oil.
Containing the preparation method of the ultra low volume liquids of fluacrypyrim composition, under normal temperature and pressure, in the reaction vessel that band stirs, take raw material according to percentage by weight, first drop in reactor by carrier, low whipping speed is drop into active ingredient under 60 ~ 80 revs/min of conditions, after active ingredient is dissolved completely, input table surface-active agent, stirs 15 ~ 30 minutes, can obtain the ultra low volume liquids containing fluacrypyrim composition of the oily of homogeneous transparent.
A kind of ultra low volume liquids containing fluacrypyrim of the present invention adopts ultra low volume spraying, low-gallonage spraying or electrostatic spray, can be used for control oranges and tangerines, apple evil mite.
Technique effect of the present invention is: the ultra low volume liquids containing fluacrypyrim of the present invention compared with prior art, has the following advantages: 1) mu spray amount is low, 60 ~ 330mL, be conventional spraying consumption hundreds of/mono-, work efficiency is high; 2) droplet is thin, ultra low volume liquids particle size range 20 ~ 100 μm, and conventional fogdrop diameter 200 ~ 600 μm, and easily stick to crops or pest surface, good penetrability, biologically active is high, and quick-acting is good; 3) more resistance of rainwater washing against, the lasting period is long; 4) safety is high; 5) the elegant loss of droplet is little, and agricultural chemicals availability is high, and environmental pollution is little; 6) be easy to packaging and use, production, storage, transportation safety.
Embodiment
Following specific embodiment is for further describing the present invention, but the present invention is only limitted to absolutely not these examples.In embodiment, each component percentages or proportioning are all by weight.Active component in each formula calculates with effective content.
Embodiment one
Adopt 4% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 1 part of fluacrypyrim, 3 parts of Bifenazates, 10 parts of 1-METHYLPYRROLIDONEs, 15 parts of solvent naphtha 150# are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add 6 parts of agriculture breast OX-2681,4 parts of agriculture breast OX-8686,3 parts of agriculture breast 500#, 2 parts of agriculture breasts 1601, triacetyl glycerines complement to 100%, stir 30 minutes, 4% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
Embodiment two
Adopt 12% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 4 parts of fluacrypyrims, 8 parts of Bifenazates, 10 parts of tetraethyleneglycol dimethyl ethers, 8 parts of diethylene glycol monoethyl ethers are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add 6 parts of agriculture breasts, 2201,4 parts of agriculture breast 0201B, 3 parts of agriculture breast 500#, 2 parts of agriculture breast S80, castor oil methyl esters complement to 100%, stir 30 minutes, 12% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
Embodiment three
Adopt 20% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 5 parts of fluacrypyrims, 15 parts of Bifenazates, 10 parts of diethylene glycol diethyl ethers, 10 parts of repefrals are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add 5 parts of polyoxyethylene (n20) phenethyl phenol ether through reaction oleates, 6 parts of agriculture breasts 507,3 parts of agriculture breast OX-635,2 parts of agriculture breasts 1601, ethylene sebacates complement to 100%, stir 30 minutes, 20% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
Embodiment four
Adopt 40% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 10 parts of fluacrypyrims, 30 parts of Bifenazates, 20 parts of diethylene glycol monoethyl ethers, 10 parts of solvent naphtha D80 are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add the newborn LME-2 of 6 parts of agriculture breasts, 2201,4 parts of agricultures, 4 parts of agriculture breast OX-8686,2 parts of agriculture breasts 1601, diethyl maleates complement to 100%, stir 30 minutes, 40% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
Embodiment five
Adopt 32% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 8 parts of fluacrypyrims, 24 parts of Bifenazates, 10 parts of diethylene glycol monobutyl ethers, 20 parts of diethylene glycol acetates are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add 7 parts of polyoxyethylene (n20) phenethyl phenol ether through reaction oleates, 5 parts of agriculture breasts 2201,4 parts of agriculture breast OX-690, triacetyl glycerines complement to 100%, stir 30 minutes, 32% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
Embodiment six
Adopt 36% fluacrypyrim Bifenazate ultra low volume liquids.By recipe requirements, at normal temperatures and pressures, 9 parts of fluacrypyrims, 27 parts of Bifenazates, 10 parts of 1-METHYLPYRROLIDONEs, 20 parts of solvent naphtha D80 are added in mixing kettle, be uniformly mixed, active ingredient is made to be dissolved into homogeneous oil phase, then add the newborn 0201B of 8 parts of agriculture breasts, 2201,5 parts of agricultures, 3 parts of agriculture breast OX-8686,2 parts of agriculture breasts 1601, diethylene glycol monoethyl ethers complement to 100%, stir 30 minutes, 36% fluacrypyrim Bifenazate ultra low volume liquids of homogeneous transparent can be obtained.
The above-mentioned prepared ultra low volume liquids containing fluacrypyrim composition, outward appearance is homogeneous oily liquids, under-5 DEG C of conditions, refrigeration 7d, nodeless mesh and suspension are separated out; Heat storage (54 ± 2) DEG C/14 days, active ingredient resolution ratio is all less than 5%; Volatility is low, and filter paper hangs sends out measurement result, and volatility is lower than 30%; To plant safety, without poisoning; Employing method of remaining silent measures, and flash-point is greater than 60 DEG C; Viscosity is less than 30mPas.
Embodiment seven, biological activity test embodiment
The active comparative trial of indoor biological, test medication liquid making method: accurately take reagent agent respectively with electronic analytical balance, respectively two kinds of former medicines are added after appropriate solvent dissolves completely, desired concn mother liquor is mixed with the water containing 0.1% Tween 80, by two kinds of active ingredient mother liquors in proportion (number based on active component weight is 1: 3) be hybridly prepared into mixed solution, be diluted to the serial liquid of tool finite concentration gradient respectively by experimental scheme dosage.
Test method: the test sample adopting potted plant seedling spray-on process to measure different batches becomes the active size of mite to Tetranychus cinnabarinus.First becoming mite to receive Tetranychus cinnabarinus of the same size is on the Tolerance of Kidney Bean Seedlings blade of first pair of true leaf open and flat phase, after becoming mite stable, count radix; Then by the order even spraying of experimental scheme from low dosage to high dose, every strain 2mL, often processes and repeats for 3 times, separately establish blank.Examination material after process is placed in the observation ward of certain condition, periodic investigation becomes mite number anyway, calculates lethality.
Table 1 section Example formulation samples acaricidal activity measurement result
Embodiment eight, field control effectiveness test
The furthermore bright beneficial effect of the present invention of field efficacy measurement result that carries out of the connected applications embodiment of the present invention more below.
Test site: Xian District, Shanxi Province suburban area;
Controlling object: phyllocoptruta oleivora;
Test with medicament: the embodiment of the present invention (Shanxi Lvhai Pesticide Technology Co., Ltd. researches and develops, provides), contrast medicament: 40% fluacrypyrim Bifenazate suspending agent (commercial), 30% fluacrypyrim suspending agent (commercial), 43% Bifenazate suspending agent (commercial).
Test arrangement: each community 2-3 fruit tree, establishes protection row around, repeats 4 times; 3 days, 7 days, 14 days, 30 days investigation preventive effects after medicine, the method of investigation drug effect is: 2 strain trees are investigated in each community, 2, killed blade or the fruit 2 of same tip phase is respectively marked in east, south, west, north, the middle direction of tree, often some investigation 2 to 3 visuals field, calculate mite number of living, if harm is comparatively light, sampling survey quantity can be increased.Result of the test is as table 2:
The control efficiency of table 2 pair phyllocoptruta oleivora
As can be seen from Table 2: adopt ultra low volume liquids of the present invention by ultra low volume spraying method control field citrus red mite, its effect is stronger than contrast medicament conventional sample spraying quick-acting, control efficiency good, synergy is obvious, the lasting period is longer.According to the observation to field trial process whole process, within the scope of test dose, mandarin tree grows fine, and poisoning phenomenon does not all appear in each treatment agent, illustrates that formulation products of the present invention is safe to oranges and tangerines.
Last it is noted that obviously, above-described embodiment is only for example of the present invention is clearly described, and the restriction not to embodiment.For those of ordinary skill in the field, can also make other changes in different forms on the basis of the above description.Here exhaustive without the need to also giving all embodiments.And thus the apparent change of amplifying out or variation be still among protection scope of the present invention.
Claims (4)
1., containing the ultra low volume liquids of fluacrypyrim composition, it is characterized in that, said composition forms by by active component, surfactant and carrier, and the weight percentage of each component is: active component 1 ~ 50%, surfactant 5 ~ 30%, surplus are carrier; Wherein, active component is fluacrypyrim, Bifenazate, and the two relative scale is 1: 3 based on the number of active component weight.
2. as claimed in claim 1 containing the ultra low volume liquids of fluacrypyrim composition, it is characterized in that, described surfactant is following one or at least two kinds of mixtures: ethoxylated castor oil, polyoxyethylene (n20) phenethyl phenol ether through reaction oleate, alkylaryl polyoxyethylene poly-oxygen propylene aether, alkylphenol polyoxyethylene phosphate, phenethyl phenol polyethenoxy ether phosphate, alkylaryl formaldehyde resin APEO, triphenyl vinyl phenol polyoxyethylene (n
20) ether phosphoric acid triethanolamine salt, castor oil polyoxyethylene ether, Ben-zylphenol Polyoxyethyl Ether, diphenyl phenolic group polyoxyethylene (n
18) ether formaldehyde condensation products, agriculture breast Atlox 4838B, agriculture breast Atlox 4914, agriculture breast Atsurf 3300B, agriculture breast Atlas 65000, agriculture breast LEW-O, agriculture breast LME-2, agriculture breast LME-4, agriculture breast LME-5, agriculture breast LEW-5, agriculture breast LEW-50, agriculture breast PICO-LE25, agriculture breast AEO-3, agriculture breast 0201B, agriculture breast 0203B, agriculture breast T-20, agriculture breast T-80, agriculture breast T-85, agriculture breast S-80, agriculture breast 507#, agriculture breast 100#, agriculture breast 36#, agriculture breast 500#, agriculture breast 600#, Nongru-700 #, agriculture breast 1601#, agriculture breast OX-2681, agriculture breast 2201#, agriculture breast NP-7, agriculture breast NP-10, agriculture breast NP-15, agriculture breast OX-635, agriculture breast OX-653, agriculture breast OX-690, agriculture breast OX-8686, agriculture breast PICO-LOE, agriculture breast PICO-LE1.
3., as claimed in claim 1 containing the ultra low volume liquids of fluacrypyrim composition, it is characterized in that, described carrier is following one or at least two kinds of mixtures: diethyl malonate, pimelic acid diethylester, diethyl maleate, triacetyl glycerine, tetraethyleneglycol dimethyl ether, butyl cellosolve, diethylene glycol acetate, diethylene glycol monoethyl ether, diethylene glycol diethyl ether, diethylene glycol monobutyl ether, diethyl oxalate, ethylene sebacate, solvent naphtha 150#, solvent naphtha 180#, solvent naphtha 200#, solvent naphtha D80, repefral, dibutyl phthalate, dioctyl phthalate, o-dichlorohenzene, acetophenone, cyclohexanone, 1-METHYLPYRROLIDONE, DMF, DMA, phenmethylol, methyl-sulfoxide, diethylene glycol acetate, n-hexyl alcohol, n-octyl alcohol, Liquid Macrogol, PEG400, methyl oleate, ethyl oleate, olein, glycerin monostearate, castor oil methyl esters, triethylene Glycol ether, epoxidized soybean oil, cottonseed oil, rapeseed oil, corn oil, castor oil.
4. described in a claim 1-3 any one, contain the preparation method of the ultra low volume liquids of fluacrypyrim composition, it is characterized in that, under normal temperature and pressure, in the reaction vessel that band stirs, raw material is taken according to percentage by weight, first carrier is dropped in reactor, low whipping speed is drop into active ingredient under 60 ~ 80 revs/min of conditions, after active ingredient is dissolved completely, input table surface-active agent, stir 15 ~ 30 minutes, the ultra low volume liquids containing fluacrypyrim composition of the oily of homogeneous transparent can be obtained.
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Application publication date: 20150610 |