CN104365606B - Dihalo pyrazole amide and Tolfenpyrad complex insecticidal composition - Google Patents
Dihalo pyrazole amide and Tolfenpyrad complex insecticidal composition Download PDFInfo
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Abstract
The invention belongs to technical field of agricultural insecticide, particularly a kind of dihalo pyrazole amide and Tolfenpyrad complex insecticidal composition.Its active ingredient is dihalo pyrazole amide and Tolfenpyrad; Both weight ratios are 1:4 ~ 7, preferred 1:5.The present invention is made up of the active ingredient of different mechanism of action, and action site increases, and is conducive to overcoming and delay the drug-fast generation of insect pest, and has widened insecticidal spectrum; Drug effect increases substantially, and the preventive effect time is long, and the field rate of active ingredient declines, and reduces production and use cost, reduces residue of pesticide and environmental pollution.
Description
Technical field
The invention belongs to technical field of agricultural insecticide, particularly a kind of dihalo pyrazole amide and Tolfenpyrad complex insecticidal composition.
Background technology
Dihalo pyrazole amide is the wide derivative of health, belong to 3-halo ethyoxyl pyrazol acid amide compounds, efficiently can activate the ryanodine receptor in insect cell, combine with it, cause the improper long-time opening of this receptor passage, thus the calcium ion in excessive release cells, cause insect muscular paralysis, death of finally paralysing.Its structure is as shown in general formula I: in formula: R1 is selected from CH3, Cl or Br; R2 is selected from Cl or Br; R3 is selected from CH3, CH (CH3) 2, CH2C ≡ CH.Field efficacy finds, dihalo pyrazole amide is to striped rice borer, rice leaf roller, diamond-back moth, cotton bollworm, cabbage caterpillar, and the pest controling effects such as nocturnal moth class are remarkable.
Tolfenpyrad, English TOLFENPYRAD by name, molecular formula is C21H22ClN3O2, and molecular weight is 383.8713, CAS registration number is 129558-76-5, and sterling outward appearance is off-white color crystallization, and Tolfenpyrad is novel pyrazole heterocyclic insecticidal/acaricidal agent.Its mechanism of action is hinder the electronics in mitochondrial metabolic system to pass on system complex I, thus electronics reception and registration is hindered, and insect can not be provided and storing energy, be called as Mitochondrial electron and pass on complex Inhibitors (METI).Insecticidal spectrum is wide, has action of contace poison.Special efficacy is had to lepidopterous larvae diamond-back moth, Thysanoptera thrips.Measure through toxicity, have greater activity to diamond-back moth (2 age) and flower thrips (1 age).Through field control effectiveness test, result shows that Tolfenpyrad 15% missible oil has good preventive effect to brassicaceous vegetable diamond-back moth, eggplant thrips.
In the real process of agricultural production, using chemical agent is the most effective means of control plant pest, but is the generation of pest resistance to insecticide by the problem that chemical control insect the most easily produces.And use single chemical insecticide continuously for a long time high dose, composite or the mixture of the rational chemical insecticides of series of problems such as residual, the environmental pollution of medicament is easily caused to have expansion insecticidal spectrum, improve control efficiency, extend the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce and remain, 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 solved the problem.Develop new product insecticide price constantly rises, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite and mixture has small investment, the lead time is short and be subject to domestic and international attention, numerous and confused increasing develops dynamics.
Summary of the invention
For solving the problem, the invention provides that a kind of insecticidal spectrum is wide, consumption is few, cost is low, have the complex insecticidal composition of synergistic effect.
Technical scheme of the present invention is: a kind of dihalo pyrazole amide and Tolfenpyrad complex insecticidal composition, and its active ingredient is dihalo pyrazole amide and Tolfenpyrad.
The weight ratio of described active ingredient dihalo pyrazole amide and Tolfenpyrad is 1:4 ~ 7, preferably 1: 5.
Above-mentioned active ingredient dihalo pyrazole amide and Tolfenpyrad can be buied by various commercial channel.According to the needs used, add the pesticidal preparations auxiliary elements such as pesticide field surfactant, carrier, antifreezing agent, thickener or disintegrant, composition is made wetting powder, water dispersible granules, aqueous suspension agent, oil-suspending agent or missible oil.
Described active ingredient dihalo pyrazole amide and Tolfenpyrad weight percentage are in the composition: 5% ~ 90%, preferably 30% ~ 80%.
Described pesticidal preparations auxiliary element comprises carrier and auxiliary agent.
Described carrier be one in water, solvent or filler, two kinds or three kinds, the preferred deionized water of water.
Described solvent is selected from the mixture of one or more compositions in DMF, cyclohexanone, toluene, dimethylbenzene, dimethyl sulfoxide (DMSO), methyl alcohol, ethanol, trimethylcyclohexanone, NOP, monoethanolamine, triethanolamine, isopropylamine, 1-METHYLPYRROLIDONE, propyl alcohol, butanols, ethylene glycol, diethylene glycol, ethylene glycol monomethyl ether, butyl ether, monoethanolamine, isopropylamine, methyl oleate, ethyl acetate or acetonitrile.
Described filler is selected from the mixture of one or more compositions in kaolin, diatomite, bentonite, attapulgite, white carbon, starch or precipitated calcium carbonate.
Described auxiliary agent at least comprises a kind of surfactant, according to different use occasions and demand, also can add other functional aids such as antifreezing agent, thickener, stabilizing agent, disintegrant, defoamer.
Described surfactant be selected from emulsifier, dispersant, wetting agent or bleeding agent one or more.Above-mentioned surfactant is single dose or the complex preparation of common non-ionic surface active agent or anion surfactant.
Other functional aids described to be selected from antifreezing agent, thickener, stabilizing agent, disintegrant or defoamer one or more.
Described emulsifier is selected from OP series phosphate (thermally coupled distillation columns), 600# phosphate (phenyl phenol polyoxyethylene ether phosphate), styrene polyoxyethylene ether ammonium sulfate salt, alkyl biphenyl ether disulfonic acid magnesium salts, triethanolamine salt, agriculture breast 400# (benzyl dimethyl phenol polyoxyethyl ether), Nongru-700 # (alkylphenol-formaldehyde resin polyoxyethyl ether), peaceful newborn 36# (phenethyl fluosite polyoxyethyl ether), agriculture breast 1600# (phenethyl phenol polyoxyethanyl polypropylene-base ether), ethylene oxide-propylene oxide block copolymer, OP series (polyoxyethylene nonylphenol ether), BY series (castor oil polyoxyethylene ether), agriculture breast 33# (alkylaryl polyoxyethylene poly-oxygen propylene aether), Span series (sorbitol anhydride monostearate), mixtures of one or more compositions in TWEEN Series (anhydrous sorbitol fat acid ester polyoxyethylene ether) or AEO series (fatty alcohol-polyoxyethylene ether).
Described dispersant is selected from the mixture of one or more compositions in polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkyl benzene calcium sulfonate, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic amine polyoxyethylene ether, aliphatic acid polyethenoxy ether or fatty acid glyceride APEO.
Described wetting agent is selected from the mixture of one or more compositions in lauryl sodium sulfate, neopelex, Nekal BX, wetting and penetrating agent F, spaonin powder, silkworm excrement or soapberry powder.
Described bleeding agent is selected from the mixture of one or more compositions in penetrating agent JFC (fatty alcohol-polyoxyethylene ether), penetrant t (Maleic Acid Diisooctyl sulfonate), azone or organosilicon.
Described thickener is selected from the mixture of one or more compositions in gelatin, sodium carboxymethylcellulose, hydroxyethylcellulose, Sodium Polyacrylate, modified starch, xanthans, bentonite, silica or Magnesiumaluminumsilicate.。
Described antifreezing agent is selected from the mixture of one or more compositions in ethylene glycol, propane diols, glycerine or urea.
Described defoamer is selected from the mixture of one or more compositions in silicone oil, silicone compound, C10 ~ C20 saturated fat acid compounds or C8 ~ C10 aliphatic alcohols compound.
Described disintegrant is selected from the mixture of one or more compositions in bentonite, urea, ammonium sulfate, aluminium chloride, low-substituted hydroxypropyl cellulose, lactose, citric acid, succinic acid or sodium bicarbonate.
Described stabilizing agent is selected from epoxidized soybean oil, the mixture of one or more compositions in epoxychloropropane, BHT, ethyl acetate or triphenyl phosphate.
Above-mentioned substance is all buied by various commercial channel.
Dihalo pyrazole amide of the present invention and Tolfenpyrad complex insecticidal composition, be mainly used in the various pests such as diamond-back moth, cabbage caterpillar, beet armyworm, prodenia litura, Oeobia undalis, vegetable aphid, liriomyza bryoniae, thrips, rust mite of preventing and treating on the cereal such as various vegetables, wheat and fruit tree.
Beneficial effect of the present invention is:
1, the present invention is made up of the active ingredient of different mechanism of action, action site increases, be conducive to overcoming and delay the drug-fast generation of insect pest, and widen insecticidal spectrum, be particularly suitable for the sucking pest for preventing and treating vegetables and fruit, pests with chewing mouthparts, mite class, lepidoptera pest.
2, drug effect of the present invention increases substantially, and the preventive effect time is long, and the field rate of active ingredient declines, and reduces production and use cost, reduces residue of pesticide and environmental pollution.
3, the present invention is compared with use one-component insecticide, and the risk producing poisoning reduces; Good to person poultry safety, Environmental compatibility.
4, the present invention is made up of the active ingredient that two kinds of mechanism of action is different, is conducive to avoiding drug-fast generation and delaying the drug-fast generation speed of germ.
5, the present invention is with low cost, and preparing process is simple, is applicable to large scale application.
Embodiment
The present invention is illustrated below in conjunction with embodiment.
First dihalo pyrazole amide and the composite rear co-toxicity bioassay test of Tolfenpyrad is adopted to prove that both strengthen composite rear drug effect.
One, test method
For examination target: diamond-back moth
Test medicine: the former medicine of 96% dihalo pyrazole amide, is produced by Zibo Xian Longda agricultural chemicals Co., Ltd; Tolfenpyrad, is produced by Yangzhou You Nuo Chemical Company; Dihalo pyrazole amide with Tolfenpyrad with Different Weight than composite mixture.
Test method: by appropriate dihalo pyrazole amide with Tolfenpyrad with Different Weight ratio (1:11,1:9,1:8,1:7,1:6,1:5,1:4,1:3,1:1) be made into composition, then be that each composition dissolves by solvent respectively with acetone, be made into 10000 μ g/ml mother liquors, in 4 DEG C of preservations, stand-by.
On the basis of preliminary experiment, in order to upper method respectively to single dose dihalo pyrazole amide and Tolfenpyrad toxicity test, the two EC
50value is respectively 0.48mg/l and 42.73mg/l.
Adopt blade infusion process: in the liquid prepared, soak 10S respectively by there is no the cabbage leaves of contacted any medicament, taking-up puts into culture dish after drying, each culture dish access is healthy, larva of the same size 10, and every concentration repeats for 3 times, if clear water is contrast.Be placed in temperature 23 ~ 29 DEG C, the incubator of humidity 86% cultivates, be standard survey insect population lethality to try worm stiff after 48h.
Carry out the toxicity test of mixture according to mixed ratio by single dose toxicity test method.
According to the EC of the abundant method of Sun Yun by each process of mensuration
50value is converted into actual mixed toxicity index (ATI); According to the proportioning of mixture, obtain theoretical mixed toxicity index (TTI), by the co-toxicity coefficient (CTC) of following formulae discovery mixture.
Single dose toxicity index=(standard agent EC
50/ reagent agent EC
50) X100
ATI=(standard agent EC
50/ reagent agent (using with) EC
50) X100
The content (%) of toxicity index XB in using with of content (the %)+B of toxicity index XA in using with of TII=A
CTC＝(ATI/TTI)X100
If co-toxicity coefficient large 120, shows there is synergistic effect; If be starkly lower than 100 (less than 80), be indicated as antagonism; Between 100 ~ 120, be indicated as summation action.
Result of the test is as shown in table 1, and in table, A represents dihalo pyrazole amide, and B represents Tolfenpyrad.
The co-toxicity coefficient of table 1 dihalo pyrazole amide and the composite mixture of Tolfenpyrad
| Test medicine | The mass ratio of A and B | Actual measurement poison refers to | Theoretical poison refers to | Co-toxicity coefficient | Conclusion |
| A | 1：0 | 100.00 | 100.00 | / | / |
| B | 0:1 | 1.12 | 1.12 | / | / |
| A+B is composite | 1:11 | 9.39 | 9.35 | 100.4 | Be added |
| A+B is composite | 1:9 | 12.58 | 11.01 | 114.3 | Be added |
| A+B is composite | 1:8 | 14.51 | 12.11 | 119.8 | Be added |
| A+B is composite | 1:7 | 18.40 | 13.48 | 136.5 | Synergy |
| A+B is composite | 1:6 | 26.89 | 15.25 | 176.3 | Synergy |
| A+B is composite | 1:5 | 35.44 | 17.60 | 201.4 | Synergy |
| A+B is composite | 1:4 | 32.14 | 20.90 | 153.8 | Synergy |
| A+B is composite | 1:3 | 30.80 | 25.84 | 119.2 | Be added |
| A+B is composite | 1:1 | 50.71 | 50.56 | 100.3 | Be added |
Can be found out: dihalo pyrazole amide: during Tolfenpyrad=1:4 ~ 7, co-toxicity coefficient is higher than 120, has synergistic effect, especially when 1:5, apparently higher than 120, have obvious synergistic effect by the data of table 1.Prove dihalo pyrazole amide provided by the invention and the effect of Tolfenpyrad mixture synergism obvious.
Below adopt field efficacy small plot experiment method, prove that dihalo pyrazole amide and composite the using in land for growing field crops of Tolfenpyrad have synergistic effect to desinsection further, and can use in land for growing field crops.
One, experimental condition
1, subjects and trial crops
Subjects: diamond-back moth
Trial crops: wild cabbage
2, environmental condition
Field trial is carried out being arranged in the outdoor cabbage field in Qingzhou City Dong Xia town, Shandong Province, and this field gesture is smooth, and wild cabbage growing way is basically identical.
Two, experimental scheme
1, medicament
1.1, test medicine
Select the medicament that following examples 1-4 is obtained.
1.2, medicament is contrasted
Comparative example 1 medicament: 10% dihalo pyrazole amide aqueous suspension agent
Comparative example 2 medicament: 20% Tolfenpyrad aqueous suspension agent
1.3, blank
If do not use the blank of any medicament
2, community arranges
Community arranges: the community of test medicine, contrast medicament and blank process and adopts random district group to arrange, and employing fixes a point to investigate, and fixes a point 5 strains in every community.
Number of repetition: each process repeats 4 times.
3, control time and number of times
Radix is investigated: before dispenser process
Second time investigation: after dispenser process 1d
Third time investigation: after dispenser process 3d
4th investigation: after dispenser process 7d
3.3, drug effect computational methods
Drug effect calculates as follows
4, on the impact of crop
4.1, chemical injury of crops is affected
Compared in chemicals treatment district and blank district, whether after dispenser, continuous 7d estimates medicament has poisoning to crop, evaluates poisoning: plant growth is normal, substantially affects without poisoning.
4.2, other biological is affected
On ambient water, soil, air etc. substantially without impact, Oral toxicity is tested, nontoxic to its mouse oral reality.
In following examples, percentage is all weight percentage, and the treatment dosage of field efficacy is effective ingredient consumption.
Embodiment 1:(30% dihalo pyrazole amide Tolfenpyrad aqueous suspension agent) 1:5
Component and content: dihalo pyrazole amide, 5.0%; Tolfenpyrad, 25.0%; Emulsifier agriculture breast NP-10,2%; Dispersant polycarboxylate, 3%; Thickener selects xanthans and aluminium-magnesium silicate, and consumption is respectively 0.1% and 2%; Antifreeze glycol, 5%; Defoamer silicone compound, 0.2%; Water, surplus.
Embodiment 2:(50% dihalo pyrazole amide Tolfenpyrad aqueous suspension agent) 1:4
Component and content: dihalo pyrazole amide, 10.0%; Tolfenpyrad, 40.0%; Emulsifier agriculture breast NP, 10,2%; Dispersant polycarboxylate, 3%; Thickener selects xanthans and aluminium-magnesium silicate, and consumption is respectively 0.1% and 2%; Antifreeze glycol, 5%; Defoamer silicone compound, 0.2%; Water, surplus.
The preparation method of above-described embodiment 1-2 is: the component provided by embodiment and percentage by weight thereof, dihalo pyrazole amide and Tolfenpyrad, surfactant and other functional aids are placed in reactor successively, add water and mix, through high speed shear, wet method sand milling, namely last homogeneous filtration obtains aqueous suspension agent.Capital equipment is batching kettle, colloid mill or homogeneous mixer, sand mill.
Embodiment 3:(70% dihalo pyrazole amide Tolfenpyrad water dispersible granules) 1:6
Component and content: dihalo pyrazole amide, 10%; Tolfenpyrad, 60%; Wetting agent dodecylbenzene sodium sulfonate, 3%; Dispersant alkylnaphthalene sulfonate formaldehyde condensation products, 8%; Filler attapulgite, surplus.
The preparation method of above-described embodiment 3 is: the component provided by embodiment and percentage by weight thereof, dihalo pyrazole amide, Tolfenpyrad, dispersant, wetting agent and filler are mixed, the water of 10 ~ 25% is added, then through kneading, extruder grain, oven dry i.e. obtained water dispersible granules after airslide disintegrating mill is pulverized.Maybe the powder pulverized is sprayed water in boiling granulator, granulation, drying, the afterwards obtained water dispersible granules of screening.Capital equipment has mixer, airslide disintegrating mill, kneader, Squeezinggranulator, drying room or fluid-bed drying, or boiling granulator, screening machine.
Embodiment 4:(80% dihalo pyrazole amide Tolfenpyrad wetting powder) 1:7
Component and content: dihalo pyrazole amide, 10%; Tolfenpyrad, 70%; Wetting agent lauryl sodium sulfate, 2%; Dispersant calcium lignosulfonate, 8%; Filler white carbon, 18%, filler kaolin, surplus.
The preparation method of embodiment 4 is: the component provided by embodiment and percentage by weight thereof, MTI-446, second mite azoles, dispersant, wetting agent and filler is mixed, and after airslide disintegrating mill is pulverized, mixing obtains wetting powder again.Capital equipment has mixer, airslide disintegrating mill.
Embodiment 5:(30% dihalo pyrazole amide Tolfenpyrad oil-suspending agent) 1:3
Component and content: dihalo pyrazole amide, 7.5%; Tolfenpyrad, 22.5%; Emulsifier agriculture breast BY-125,7%; Thermally coupled distillation columns 8%; Organobentonite selected by thickener, and consumption is respectively 1.6%; Methyl oleate, surplus.
The preparation method of above-described embodiment 5 is: the component provided by embodiment and percentage by weight thereof, dihalo pyrazole amide and Tolfenpyrad, surfactant and other functional aids are placed in reactor successively, add methyl oleate to mix, through high speed shear, wet method sand milling, namely last homogeneous filtration obtains oil-suspending agent.Capital equipment is batching kettle, colloid mill or homogeneous mixer, sand mill.
Embodiment 6:(36% dihalo pyrazole amide Tolfenpyrad missible oil) 1:8
Component and content: dihalo pyrazole amide, 4.0%; Tolfenpyrad, 32.0%; Agriculture breast 500# and agriculture breast OP-10# selected by emulsifier, and consumption is respectively 4% and 5%; DMF, 10% selected by solvent, ethyl acetate, 15%, dimethylbenzene, surplus.
The preparation method of above-described embodiment 6 is: the component provided by embodiment and percentage by weight thereof, dihalo pyrazole amide and Tolfenpyrad is added in solvent, and adds emulsifier wherein, is uniformly mixed being uniformly mixed in still.Be uniformly mixed still and can select enamel reaction still, stainless steel stirred tank etc.
It is as shown in table 2 that embodiment 1-4 and comparative example 1-2 prevents and treats the diamond-back moth test of pesticide effectiveness.
Table 2 embodiment 1-4 and comparative example 1-2 prevents and treats the field control effectiveness test result of diamond-back moth
As can be seen from table 2 result of the test, comparative example 1: dihalo pyrazole amide mu active ingredient: 15 × 10%=1.5 gram; Comparative example 2: Tolfenpyrad mu active ingredient: 40 × 20%=8 gram.Embodiment 1: mu active ingredient: 5 × 30%=1.5 gram.Single dose is according to the theoretical mu medication of embodiment 1 compound proportion: (1.5 × 1+8 × 5)/6=6.92 gram.The preventive effect of the active ingredient mu dosage 1.5 grams of embodiment 1 is greater than the preventive effect of single dose according to the theoretical mu medication 6.92 grams of embodiment 1 compound proportion, can judge embodiment 1 synergy.By that analogy, can draw: the control efficiency of embodiment 1-4 is all better than comparative example 1-2, when the mu consumption of composite mixture active ingredient is lower than single dose, preventive effect, still higher than single dose, shows that dihalo pyrazole amide and Tolfenpyrad compounded pesticides have obvious synergistic effect to insect.In addition, duration of test field observation, embodiment medicament respectively processes liquid on plant growth without impact, to around beneficial organism safety, good with Environmental compatibility.As can be seen here, dihalo pyrazole amide and Tolfenpyrad composite be a desirable insecticide mixture.
Claims (5)
1. dihalo pyrazole amide and a Tolfenpyrad complex insecticidal composition, is characterized in that: its active ingredient is dihalo pyrazole amide and Tolfenpyrad; The weight ratio of described active ingredient dihalo pyrazole amide and Tolfenpyrad is 1:4 ~ 7.
2. dihalo pyrazole amide according to claim 1 and Tolfenpyrad complex insecticidal composition, is characterized in that: the weight ratio of described active ingredient dihalo pyrazole amide and Tolfenpyrad is 1:5.
3. dihalo pyrazole amide according to claim 1 and Tolfenpyrad complex insecticidal composition, is characterized in that: described active ingredient dihalo pyrazole amide and Tolfenpyrad weight percentage are in the composition 5% ~ 90%.
4. dihalo pyrazole amide according to claim 3 and Tolfenpyrad complex insecticidal composition, is characterized in that: described active ingredient dihalo pyrazole amide and Tolfenpyrad weight percentage are in the composition 30% ~ 80%.
5. the dihalo pyrazole amide according to any one of Claims 1 to 4 and Tolfenpyrad complex insecticidal composition, is characterized in that, the formulation of described composition is wetting powder, water dispersible granules, aqueous suspension agent, oil-suspending agent or missible oil.
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