CN102369941B - Insecticidal and acaricidal composition containing bifenazate and chlorfenapyr - Google Patents
Insecticidal and acaricidal composition containing bifenazate and chlorfenapyr Download PDFInfo
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Abstract
The invention discloses an insecticidal and acaricidal composition containing bifenazate and chlorfenapyer, and a preparation method and application thereof. The insecticidal composition is characterized by containing bifenazate, chlorfenapyr and other auxiliary agents, wherein a mass ratio of bifenazate to chlorfenapyr is 70:1-60:1. The composition can be applied to control of various insects on various crops and is safe, environment-friendly, at low costs and with good effect. According to indoor virulence determination and field drug effect test, complex formulation of the two compounds is proved to have obvious synergism on target insects. And no report about complex formulation of bifenazate and chlorfenapyer is disclosed home or abroad, so the invention is provided.
Description
Technical field
The invention belongs to agriculture chemical compounding field, relate to a kind of insecticide acaricide composition and application thereof, especially a kind of insecticide acaricide composition and application thereof take Bifenazate and chlorfenapyr as main active.
Technical background
In the real process of agricultural production, using chemical agent is the most effectively means of control plant pest, but the problem the most easily producing by chemical control insect is the generation of pest resistance to insecticide.And long-term use single chemical insecticide continuously high dose, easily cause the series of problems such as residual, environmental pollution of medicament.Reasonably the composite or mixture of chemical insecticide has expansion insecticidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay insect evil mite drug resistance and the positive feature such as drug-fast generation and development, the composite or mixture of insecticidal/acaricidal agent is one of the effective method the most addressing the above problem.Exploitation new product insecticide price is constantly soaring, and by contrast, exploitation is efficient with research, composite and the mixture of low toxicity, low-residual has small investment, the lead time is short and be subject to domestic and international attention, and numerous and confused increasing develops dynamics.
Bifenazate (bifenazate): 3-(4-methoxyl biphenyl base-3-yl) carbazic acid isopropyl ester
Bifenazate is biphenyl hydrazine class miticide.Its sterling outward appearance is white crystalline solid; Molten point is 121.5～123.0 ℃; Vapour pressure (25 ℃): 3.8 × 10
-7pa; Solvability (20 ℃): be 2.1mg/L in water; In organic solvent (g/L): in toluene 24.7, in ethyl acetate 102, in methyl alcohol 44.7, in acetonitrile 95.6, in hexane 0.232, in 1-octanol 8.91; Distribution coefficient (n-octyl alcohol/water): Log Pow=3.5; Bifenazate is a kind of new selective foliar spray miticide.Its mechanism of action is the unique effect of γ-aminobutyric acid (GABA) acceptor of the nervous centralis conducting system to mite class.Its each life stage to mite is effective, have ovicidal activity and knock down activity (48～72h) with to what become mite, and the lasting period is long.Through Toxicity Determination and field control effectiveness test result, show, better to the control efficiency of apple tree two spotted spider mite.Dosage is 160～240mg/kg (2000～3000 times of liquid of said preparation dilution), in mite class harm initial stage foliar spray, uses.Lasting period 14d left and right, recommendation dosage range is interior to crop safety.To parasitic wasp, Predatory Mites, Chrysopa low-risk.
Chlorfenapyr (chlorfenapyr):
Have another name called capillary, external title is eliminating, and genus aryl adjoins coughs up compounds, is that in it, absorption is very strong by the chemical constitution that contains pyrrole ring natural antibiotics is transformed successfully and developed, and mutually uses non-resistant with other drug simultaneously.Insect is had to stronger stomach poison function and certain action of contace poison, its mechanism of action uniqueness, the lasting period is long, and the various pests evil mite on fruit tree, vegetables, cotton, legume crop is had to good preventive effect.Toxicity to person poultry toxicity is lower, is current quite concerned efficient pesticide-miticide.
Summary of the invention
The present invention's pleasantly surprised discovery in Toxicity Determination experiment, Bifenazate and chlorfenapyr are composite can improve the activity to insect greatly, equally the insect of Bifenazate single dose and chlorfenapyr single dose generation resistance is had to higher activity.
The present invention realizes by following measures.
A kind of insecticide acaricide composition, it contains Bifenazate and chlorfenapyr, and wherein the weight ratio of Bifenazate and chlorfenapyr is 1: 70～60: 1.
Described insecticide acaricide composition, wherein the more excellent weight ratio of Bifenazate and chlorfenapyr is 1: 50～50: 1.
Described insecticide acaricide composition, wherein to accumulate the weight ratio of shared preparation be 1～71% to two kinds of active principles of Bifenazate and chlorfenapyr.
Described insecticide acaricide composition, Bifenazate and chlorfenapyr and auxiliary agent, carrier etc. are processed into any one formulation allowing on agricultural chemicals.
Described insecticide acaricide composition, is characterized in that the formulation that can be processed into is suspending agent, aqueous emulsion, microemulsion, wetting powder, soluble powder, water dispersible granules and microcapsule formulations etc.
Described insecticide acaricide composition is for preventing and treating mite class in various crop, lepidoptera pest etc.
The insecticides with synergistic effect takes following measures to realize:
One of technical scheme of the present invention, described insecticide acaricide composition is suspending agent, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Dispersant 5～20%
Antifreezing agent 0.5～3%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
The concrete production stage of this insecticide acaricide composition suspending agent is for first mixing other auxiliary agents, through high speed shear, mix, add Bifenazate and chlorfenapyr, abrading-ball 2～3 hours in ball crusher, make a diameter all below 5mm, make the suspending agent preparation of the insecticide acaricide composition that contains Bifenazate and chlorfenapyr of the present invention.
Two of technical scheme of the present invention, described insecticide acaricide composition is aqueous emulsion, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Emulsifier 3～30%
Solvent 5～15%
Stabilizing agent 2～15%
Antifreezing agent 1～5%
Defoamer 0.1～8%
Thickener 0.2～2%
Water surplus
The concrete production stage of this insecticide acaricide composition aqueous emulsion is: first former medicine Bifenazate and chlorfenapyr, solvent and emulsifier, cosolvent are added together, make to be dissolved into uniform oil phase; By part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When reactor high speed stirs, oil phase is added to water, slowly add water until reach phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear about half an hour, form the aqueous emulsion of oil-in-water type.Make the aqueous emulsion of the insecticide acaricide composition that contains Bifenazate and chlorfenapyr.
Three of technical scheme of the present invention, described insecticide acaricide composition is microemulsion, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Solvent 1～30%
Emulsifier 3～30%
Stabilizing agent 2～15%
Synergist 2～10%
Water 10～78%
The concrete procedure of processing of this insecticide acaricide composition microemulsion is: Bifenazate and the former medicine of chlorfenapyr are added in solvent, add while stirring the auxiliary agents such as emulsifier, stabilizing agent and synergist, finally be added to the water stirring, formed transparent and homogeneous liquid, obtained the microemulsion of the present composition.
Four of technical scheme of the present invention, described insecticide acaricide composition is wetting powder, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Dispersant 3～20%
Wetting agent 3～10%
Filler 10～70%
The concrete procedure of processing of this insecticide acaricide composition wetting powder is: by above-mentioned formula, Bifenazate and chlorfenapyr and dispersant, wetting agent and filler are mixed, uniform stirring in stirred tank, after airslide disintegrating mill, mixing, can be made into the wetting powder of the present composition.
Five of technical scheme of the present invention, described insecticide acaricide composition is soluble powder, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Dispersant 3～20%
Stabilizing agent 3～10%
Adhesive agent 1～5%
Filler 10～70%
The concrete procedure of processing of this Herbicidal combinations soluble powder is: by above-mentioned formula, Bifenazate and chlorfenapyr and dispersant, stabilizing agent, adhesive agent and filler are mixed, uniform stirring in stirred tank, after airslide disintegrating mill, mixing, can be made into the soluble powder of the present composition.
Six of technical scheme of the present invention, described insecticide acaricide composition is water dispersible granules, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Dispersant 3～20%
Wetting agent 3～10%
Disintegrant 2～5%
Filler 10～70%
The concrete procedure of processing of this insecticide acaricide composition water dispersible granules is: by above-mentioned formula, Bifenazate, chlorfenapyr and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and in fluidized bed prilling dryer, carry out after granulation, dry, screening, through sample analysis, making the water dispersible granules of the insecticide acaricide composition that contains Bifenazate and chlorfenapyr of the present invention.
Seven of technical scheme of the present invention, described insecticide acaricide composition is microcapsule formulations, the percentage by weight of component is:
Bifenazate 1～60%
Chlorfenapyr 1～70%
Urea 5～20%
Formaldehyde 5～20%
Emulsifying dispersant 5～20%
Antifreezing agent 1～5%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
This insecticide acaricide composition microcapsule formulations procedure of processing is: in the there-necked flask that agitating device is housed, add urea and formaldehyde (amount of substance ratio be about 1: 1.5～2.0), with the left and right, pH value to 8～9 of sodium hydroxide solution regulator solution, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of Bifenazate and chlorfenapyr is dissolved in cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, is made into the O/W type stable emulsion take the aqueous solution containing emulsifying dispersant as water.Above-mentioned urea resin prepolymer is added in emulsion, regulate pH value, polymerization reaction take place under acid catalysis condition, is wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Selection adds appropriate auxiliary agent, the microcapsule suspending agent that gets final product stablely.
Described emulsifier is selected from any one or more mixtures with arbitrary proportion composition in calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styrylphenol polyoxyethylene ether, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, polyoxyethylene aliphatic alcohol ether.
Described dispersant is selected from one or more in polycarboxylate, sodium lignin sulfonate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic acid polyethenoxy ether, polyoxyethylene carboxylate, fatty acid glyceride APEO.
Described solvent is any one or more mixed solvents with arbitrary proportion composition in dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), water equal solvent.
Described wetting agent is selected from: one or more in lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, wetting and penetrating agent F, alkylnaphthalene sulfonate, alkylphenol ethoxylate, polyoxyethylene triphenylethylene phosphenylic acid salt, spaonin powder, silkworm excrement, soapberry powder.
Described synergist refers to have the medicament of enhancing penetration, wetting extended capability, knock down insect speed, improve the resistance of rainwater washing against power of agricultural chemicals, thereby improve a class safety, environmental protection of agricultural insecticide effect, the New-type adjuvant of nontoxic, noresidue, optional any in organic silicon pesticide synergist ZC-650 or organic silicon pesticide bleeding agent spreading agent Agrowet810c, agricultural organic silicon pesticide synergist Silwet408, azone.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, sodium bicarbonate.
Described thickener is selected from: one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate, polyvinyl alcohol.
Described antimicrobial is selected from: one or both in Sodium Benzoate, sodium salicylate, sodium sorbate.
Described stabilizing agent is selected from: the one in sodium citrate, resorcinol, oxirane.
Described antifreeze is selected from: one or more in ethylene glycol, propane diols, glycerine, diethylene glycol (DEG), triethylene glycol.
Described defoamer is selected from: silicone oil, silicone compound, C
10-20saturated fat acid compounds, C
8-10one or more in aliphatic alcohols compound and polyoxyethylene glycerol ether.
Described emulsifying dispersant comprises: wetting agent, dispersant, stabilizing agent, thickener, defoamer and antifreezing agent etc.
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, precipitated calcium carbonate.
The invention has the beneficial effects as follows:
1, the present invention's Bifenazate used is pyrrole insecticides, differ greatly with the anabasine insecticide chlorfenapyr mechanism of action, and without cross resistance.
2, two kinds of composite insecticide double action mechanism, can delay the generation of pest resistance to insecticide.
3, reduce agricultural chemicals usage amount, strengthened the friendly to environment.
Embodiment: Bifenazate proportioning co-toxicities different from chlorfenapyr
1.1 reagent agent
The former medicine of 97% Bifenazate, the former medicine of 94% chlorfenapyr, above-mentioned former medicine provides by Qingdao Hailir Pesticides and Chemical Co., Ltd..
1.2 for examination worm source
Examination mite is picked up from Citrus Research Institute Of Chinese Academy Of Agricultural Sciences test site, cultivation management term harmonization, do not use in the recent period medicament, adopt the blade that rewinds citrus red mite (crm), standby after normal temperature laboratory (25 ℃ of left and right) raised for 2 generations by fresh citrus leaves down.
1.3 single dose assay method slide infusion processes
The female mite that Individual Size is consistent, body colour is scarlet if choose, with writing brush by examination the mite back side stick in posting on the slide of cloth insertion sheet, every slide dilution intervals, on the basis of prerun, respectively two kinds of former medicines are dissolved in to acetone, with the 0.1% Tween 80 aqueous solution, be diluted to 5 concentration gradient liquids again, be placed in beaker standby.The glutinous slide that has an examination mite is immersed in good liquid 5 seconds, four repetitions of each processing, take out be tiltedly put in porcelain dish edge dry after, be put in Glass carrier box, do not add a cover the illumination box of putting into (25 ± 1) ℃, humidity 70%～80%, illumination every day 10 hours, microscopy mite number (with its foot of fine, soft fur style of writing, nonresponder is dead) anyway after 24 hours.The average correction lethality of examination mite is converted into probit value (Y), and concentration for the treatment of (mg/L) converts logarithm value (x) to, with method of least squares, draws virulence regression equation Y=a+bx, calculates LC
50standard error equivalence.Press the computational methods of Sun Yunpei and calculate co-toxicity coefficient CTC.
The joint toxicity measuring method of 1.4 different proportionings
According to the toxicity test result of single dose, in total active ingredient, be 20% quality than chlorfenapyr: the ratio that Bifenazate is respectively 10: 10,8: 12,6: 14,4: 16,2: 18 is carried out mixture.Adopt above-mentioned 1.3 methods to carry out toxicity test, calculate LC
50, and press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).Co-toxicity coefficient CTC, computing formula is as follows: (take Bifenazate as standard medicament, its toxicity index is 100):
The LC of actual toxicity index (ATI)=Bifenazate of M
50the LC of/M
50× 100
TI × P chlorfenapyr of TI × P Bifenazate+chlorfenapyr of theoretical toxicity index (TTI)=Bifenazate of M
TTI × 100 of the ATI/M of co-toxicity coefficient (CTC)=M of M
In formula: M is chlorfenapyr and the mixture of the different proportionings of Bifenazate
P chlorfenapyr is chlorfenapyr shared ratio in mixture
P Bifenazate is Bifenazate shared ratio in mixture
2.1 toxicity test results
Bifenazate, the indoor measurement result of chlorfenapyr to citrus red mite (crm)
As can be seen from the table, in the mixture of different proportion, its co-toxicity coefficient is all greater than 120, shows certain synergistic effect, wherein chlorfenapyr: the synergistic effect that Bifenazate is 6: 14 is the most obvious, and co-toxicity coefficient is 157.78.Result of the test shows, under indoor conditions, chlorfenapyr, two kinds of medicaments of Bifenazate all have higher activity to tangerine Panonychus citri.The result of the test of different proportion proportioning shows, by active ingredient chlorfenapyr: Bifenazate is 10: 10,8: 12,6: 14,4: 16,2: 18 o'clock, all show stronger synergistic effect, wherein take chlorfenapyr: Bifenazate is, synergistic effect is best at 6: 14 o'clock.Suggestion is carried out further field control effectiveness test to the mixture preparation of 6: 14 left and right scopes of suitable proportion, to evaluate its field practical application effect.
3.1 field experiments are surveyed panonychus citri, European red mite
3.1 field experiments are surveyed panonychus citri, European red mite (two experimental techniques are identical)
3.1 test method
3.1.1 application method
Panonychus citri experimental establishment is carried out at Zhijiang City, Hubei Province precious jade China citrus orchard.On May 6th, 2010, to June 10, carried out, European red mite experimental establishment is carried out in Liquan apple Zhu Zai district, Xianyang, Shanxi province city, on June 20th, 2010 to July 23, carries out.
While making up a prescription, after first medicament fully being dissolved with a small amount of water, then carry out complete stool spraying processing after adding suitable quantity of water, community spouting liquid is used by 675 liters/hectare, only sprays medicine one time.Spraying equipment is WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out routine spraying, makes every effort to evenly thoughtful during spray medicine.
3.1.2 investigation method
Each community is at East, West, South, North, the tender tip of middle five positions mark of every strain tree, investigate altogether 25 movable mite quantity on leaf, hand magnifier is directly observed blade face, before medicine, investigate mite mouth radix, after medicine, 1d, 3d, 7d, 14d, 21d, 28d investigate respectively the remaining mite number alive in each community, calculate mite mouth decline rate, and contrast decline rate comparison, calculating relative control effect.
3.1.3 drug effect computational methods
Mite number × 100 before decline rate (%)=(mite number after front mite number one dispenser of dispenser)/dispenser
Proofread and correct decline rate or preventive effect (%)=(treatment region mite mouth decline rate-check plot mite mouth decline rate)/(1-check plot mite mouth decline rate) × 100
3.1.4 poisoning investigation method
After dispenser, whether 14d range estimation medicament has poisoning to crop continuously.
3.2 field control effectiveness test result of the tests
Table 2 treatment agent control citrus red mite (crm) field control effectiveness test result
As can be seen from Table 2, the Mixed Pharmacy of different proportion, by different consumptions, carry out field experiment, after medicine, each investigation all shows it control efficiency of panonychus citri is all better than contrasting medicament, after dispenser 3 days, 20% (chlorfenapyr: Bifenazate) (6: 14), 7 days, 14 days, the control efficiency of panonychus citri was obviously better than to 2 contrast medicaments in 28 days, and the miticidal effect of two contrast medicament the inside 50% Bifenazate SC is also relatively good.According to the observation to field experiment 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 it is safe to oranges and tangerines.In process of the test, testing crew finds that the evil mites such as its rust mite (blister mite) all have fine preventive effect.
Table 3 treatment agent control European red mite field control effectiveness test result
As can be seen from Table 3, the Mixed Pharmacy of different proportion, by different consumptions, carry out field experiment, after medicine, each investigation all shows it control efficiency of European red mite is all better than contrasting medicament, after dispenser 3 days, 20% (chlorfenapyr: Bifenazate) (6: 14), 7 days, 14 days, the control efficiency of European red mite was obviously better than to 2 contrast medicaments in 28 days.According to the observation to field experiment process whole process, within the scope of test dose, apple tree grows fine, and poisoning phenomenon does not all appear in each treatment agent, illustrates that it is safe to apple.
To sum up described in twice field experiment result, the Pesticidal combination that the present invention contains Bifenazate and chlorfenapyr, because of these two composition mechanism of action uniquenesses, Bifenazate is effective to each life stage of mite, there is ovicidal activity and knock down activity (48～72h) with to what become mite, the lasting period of chlorfenapyr is long, can avoid the factor of Bifenazate lasting period shorter (14d left and right), the two composite phenomenon that can effectively solve fruit district evil mite " difficult beating ".Recommendation dosage range is interior to crop safety.To parasitic wasp, Predatory Mites, Chrysopa low-risk.This technology is to panonychus citri, oranges and tangerines blister mite; scale insect; the insects such as European red mite show good control efficiency; to target crop safety; compared with single dose; it is few that Pesticidal combination of the present invention has dosage; instant effect, lasting period are grown (checking can reach more than 30 days through field experiment), delay the advantage that pest resistance to insecticide produces; so; research and development of the present invention and promote the raising of fruit quality to vast fruit tree producing region, orchard worker get rich and the protection tool of local environment is of great significance.
Claims (4)
1. a Pesticidal combination, is characterized in that: the active ingredient of this Pesticidal combination is Biphenthrin and chlorfenapyr, and wherein the mass ratio of chlorfenapyr and Bifenazate is 2～10:18～10.
2. Pesticidal combination according to claim 1, is characterized in that: Biphenthrin and the chlorfenapyr gross mass in preparation accounts for 2～71% of the whole quality of the pharmaceutical preparations.
3. Pesticidal combination according to claim 1, is characterized in that: Biphenthrin and chlorfenapyr and auxiliary agent and cosolvent are re-dubbed any one formulation allowing on agricultural chemicals.
4. according to the Pesticidal combination described in claim 1 or 2 or 3, it is characterized in that: the formulation of this Pesticidal combination is suspending agent, aqueous emulsion, microemulsion, wetting powder, water dispersible granules and microcapsule formulations.
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