CN102113496B - Bactericidal composition containing dicyclanil and methomyl - Google Patents
Bactericidal composition containing dicyclanil and methomyl Download PDFInfo
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Abstract
The invention discloses a bactericidal composition containing dicyclanil and methomyl as well as a preparation method and application thereof. The bactericidal composition is characterized by containing the dicyclanil, the methomyl and other auxiliaries, wherein the weight ratio of the dicyclanil to the methomyl is (0.1-40):(0.1-40). The bactericidal composition can be used for controlling various lepidoptera pests, has the advantages of safety, environmental friendliness, low cost and good effect, and has an obvious synergistic effect based on the evidences from an indoor virulence test and a field test. In addition, the invention is proposed on the premise that no report related to blending of the dicyclanil and the methomyl exists in China and abroad.
Description
Technical field
The invention belongs to field of agrochemicals, relate to a kind of complex insecticidal composition and application thereof, especially a kind of Pesticidal combination and application thereof take CGA 183893 and Methomyl as main active.
Background technology
In the real process of agricultural production, use chemical agent and be the most effectively means of control plant pest, but by the chemical control insect the problem of easy generation be the generation of pest resistance to insecticide.And long-term use single chemical insecticide continuously high dose, cause easily the series of problems such as residual, environmental pollution of medicament.Reasonably chemical insecticide is composite or be mixed and have the expansion insecticidal spectrum, improve control efficiency, prolong the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay pest resistance and the positive characteristics such as drug-fast generation and development, pesticide compositional or to be mixed be the most one of the effective method that addresses the above problem.Exploitation new product insecticide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed have small investment, the lead time is short and be subject to domestic and international attention, the numerous and confused dynamics that develops that strengthens.
CGA 183893: 4,6-diaminourea-2-cyclopropylamino-5-cyanopyrimidine
Chemical formula: C
8H
10N
6Molecular weight: 190.21 fusing points: 249～251
This product is the aminopyrimidine insecticide, thereby main biochemical synthetic by the amino acid that suppresses dihydrofoilic acid ester reductase destruction insect.The evils such as tobacco leaf noctuid, the cotton boll that it can prevent and treat the crops such as cotton, corn, paddy rice, vegetables resembles, brown plant-hopper, rice leafhopper
Methomyl: 1-(methyl mercapto) ethylidene aminomethyl carbamate
For the high malicious insecticide of never poison, suppress the synthetic of insect acetylcholinesterase, and its high volatility, toxicity on inhalation is high, and eyes and skin are had the minimal irritation effect, under test dose without teratogenesis, mutagenesis, carcinogenesis, without chronic toxicity, poisonous to bird, honeybee, fish.The formulation that can be processed into is missible oil, aqua, wetting powder etc.Methomyl has tags and stomach poison function, without interior suction, fumigation action, has certain ovicidal effect, and the insect that organic phosphor has been produced resistance also has favorable effect.Be applicable to prevent and treat on cotton, vegetables, the tobacco Lepidoptera, Homoptera, coleoptera and other insects.
Summary of the invention
The object of the present invention is to provide a kind of component reasonable, have the complex preparation of notable synergistic effect, and can produce high insecticidal effect, drug cost is low, and can delay the resistance of insecticide.
Characteristics of the present invention are composite with suppressing insect biochemical synthetic material and never poison, and the mechanism of action of two kinds of medicines is different, and without cross resistance, through evidence, what relate in of the present invention compositely has an obvious synergistic effect.
Two kinds of its mass percents of agriculture chemical compounding composition that the present invention relates to are 0.1～40: 0.1～40, more high quality ratio is 1～40: 1: 40, and this complex composition can be processed into formulation through relevant art and missible oil arranged, the formulations such as suspending agent, aqueous emulsion, water dispersible granules, microcapsule formulations and wetting powder.
One of technical scheme of the present invention, described Pesticidal combination are cream preparation, and the percentage by weight of component is:
CGA 183893 1～40%
Methomyl 1～40%
Conventional emulsifier 10～30%
Conventional solvent 20～50%
Conventional synergist 1～5%
The concrete production stage of this cream preparation adds the stir oily liquids of rear one-tenth transparent and homogeneous of emulsifier, synergist after the fully dissolving again for first CGA 183893, Methomyl being added in the solvent, can namely makes the cream preparation that contains CGA 183893 Methomyl Pesticidal combination of the present invention.
Two of technical scheme of the present invention, described Pesticidal combination are suspending agent, and the percentage by weight of component is:
CGA 183893 1～40%
Methomyl 1～40%
Dispersant 5～20%
Antifreezing agent 1～5%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
The concrete production stage of this suspending agent is for mixing other auxiliary agents first, mix through high speed shear, add CGA 183893, Methomyl, abrading-ball is 2～3 hours in ball crusher, make a diameter all below 5mm, make the suspending agent preparation that contains CGA 183893 Methomyl Pesticidal combination of the present invention.
Three of technical scheme of the present invention, described Pesticidal combination are aqueous emulsion, and the percentage by weight of component is:
CGA 183893 1～40%
Methomyl 1～40%
Emulsifier 3～30%
Solvent 5～15%
Cosolvent 5～20%
Antimicrobial 0.1～1%
Stabilizing agent 2～15%
Antifreezing agent 2～5%
Defoamer 0.1～8%
Thickener 0.2～2%
Water surplus
The concrete production stage of this aqueous emulsion is: at first former medicine CGA 183893 and Methomyl, solvent and emulsifier, cosolvent are added together, make and be dissolved into uniform oil phase; With part water, antifreeze, other the insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water until reach the phase inversion point, open clipper and carry out high speed shear, and add remaining water, shear approximately half an hour, form the aqueous emulsion of oil-in-water type.Namely make the aqueous emulsion that contains CGA 183893 Methomyl Pesticidal combination.
Four of technical scheme of the present invention, described Pesticidal combination are water dispersible granules, and the percentage by weight of component is:
CGA 183893 1～40%,
Methomyl 1～40%
Dispersant 3～10%
Wetting agent 1～10%
Disintegrant 1～5%
The filler surplus.
The concrete production stage of this water dispersible granules is: by above-mentioned prescription CGA 183893, Methomyl and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, then add and carry out granulation, drying, screening in the fluidized bed prilling dryer by sample analysis, make the water dispersible granules that contains CGA 183893 Methomyl Pesticidal combination of the present invention.
Five of technical solution of the present invention, described Pesticidal combination are microcapsule formulations, and the percentage by weight of component is:
CGA 183893 1～40%
Methomyl 1～40%
Urea 5～20%
Formaldehyde 10～30%
Emulsifying dispersant 5～20%
Antifreezing agent 1～5%
Thickener 0.1～2%
Defoamer 0.1～0.8%
Water surplus
In being housed, the there-necked flask of agitating device adds urea and formaldehyde (molar ratio be about 1: 1.5～2.0), with the pH value to 8 of sodium hydroxide solution regulator solution～about 9, then be warming up to 70～80 ℃, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of CGA 183893 and Methomyl is dissolved in the cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, and the aqueous solution that is made into to contain emulsifying dispersant is the O/W type stable emulsion of water.Above-mentioned urea resin prepolymer is added in the emulsion, regulate the pH value, polymerization reaction take place under the acid catalysis condition is wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40～50 ℃, hardening time 1h.Select to add an amount of auxiliary agent, the microcapsule suspending agent that gets final product stablely.
Six of technical scheme of the present invention, described Pesticidal combination is wetting powder, the percentage by weight of component is:
CGA 183893 1～40%
Methomyl 1～40%
Dispersant 3～10%
Wetting agent 1～5%
The filler surplus.
The concrete production stage of this wetting powder is: by above-mentioned prescription CGA 183893, Methomyl and dispersant, wetting agent and filler are mixed, uniform stirring in stirred tank, behind airslide disintegrating mill, mix again, namely can be made into the wetting powder of the present composition.
Described conventional emulsifier is selected from any one or more mixtures that form with arbitrary proportion 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, the polyoxyethylene aliphatic alcohol ether.
Described conventional solvent is any one or more mixed solvents that form with arbitrary proportion in dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), the water equal solvent.
Described conventional synergist refers to have enhancing medicament 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, bactericidal effect, the New-type adjuvant of nontoxic, noresidue, optional in organic silicon pesticide synergist ZC-650 or organic silicon pesticide bleeding agent spreading agent Agrowet810c, agricultural organic silicon pesticide synergist Silwet408, azone any.
Described dispersant is selected from one or more in polycarboxylate, lignosulfonates, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic amine polyoxyethylene ether, polyoxyethylene carboxylate, the fatty acid glyceride APEO.
Described wetting agent is selected from: lauryl sodium sulfate, DBSA, Nekal BX., among the wetting and penetrating agent F, alkylnaphthalene sulfonate, polyoxyethylene triphenylethylene phosphenylic acid salt, spaonin powder, silkworm excrement, soapberry powder one or more.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate.
Described thickener is selected from: one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate, the polyvinyl alcohol.
Described antifreeze is selected from: one or more in ethylene glycol, propane diols, the glycerine.
Described stabilizing agent is selected from: pentaerythrite, xylitol, mannitol a kind of.
Described antimicrobial is selected from: one or both in Sodium Benzoate, sodium salicylate, the sodium sorbate.
Described defoamer is selected from: silicone oil, silicone compound, C
10-20Saturated fat acid compounds, C
8-10In the aliphatic alcohols compound one or more.
Described emulsifying dispersant comprises: dispersant, wetting agent, antimicrobial, stabilizing agent, thickener, defoamer and antifreezing agent etc.
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate.
The present invention has following features:
1. double action mechanism, insect are difficult for producing resistance;
2. synergistic effect is obvious, component of the present invention is reasonable, drug effect is high, use cost is low, synergistic effect is obvious, the present invention compares with single dose rice grub such as striped rice borer, rice fulgorid and rice leaf roller etc. has higher drug effect, and can effectively prevent and treat the primary pests such as diamond-back moth, beet armyworm on fruit tree, the vegetables;
3. active ingredient CGA 183893 and conventional carbamates is composite, and the insect that conventional pesticide is produced resistance has very high drug effect equally;
Application Example
The different proportioning co-toxicities from CGA 183893 of Methomyl
1.1 reagent agent
The former medicine of 95% Methomyl, the former medicine of 90% CGA 183893, Methomyl and CGA 183893 different proportion mixture, above-mentioned former medicine provides by Hunan Chemical Research Institute's pesticide research.
1.2 for examination worm source
Cotton bollworm (Heliothis armigera) third-instar larvae.
1.3 two single dose Toxicity Determination
Adopt drop method.On the basis of preliminary experiment, Methomyl is become 7 series concentration by certain gradient with acetone diluted respectively with CGA 183893, concentration range is located at and can causes for the examination insect mortality between 10%～90%.With micro intravenous drip instrument liquid is pursued a drop in the chest and back of cotton bollworm third-instar larvae, every larva point drops physic liquor 0.5 * 2ul, the larva after the processing is put into dactylethrae, feeds with a small amount of cotton leaf, and a dactylethrae is put 1 larva.Each concentration is processed 30, repeats 3 times, and other compares with the acetone drop, moves into afterwards in 25 ± 1 ℃ the incubator.Check after 48 hours and respectively process dead borer population, lethality Abbott formula correction, again according to the concentration logarithm---the lethality probit value is analyzed (Bliss) method, the value of obtaining virulence regression equation and putting dead middle amount LD50.
2.1 best proportioning screening
Mix in proportion the optimizing that is mixed of (Crafte) method, filter out the best proportioning that Methomyl and CGA 183893 are mixed.If Methomyl and CGA 183893 are respectively a and b to 48 hours indoor virulence LD50 of cotton bollworm third-instar larvae, be mixed into 11 prescriptions in following ratio when two medicaments are mixed, be a+0,0.9a+0.1b, 0.8a+0.2b, 0.7a+0.3b, 0.6a+0.4b, 0.5a+0.5b, 0.4a+0.6b, 0.3a+0.7b, 0.2a+0.8b, 0.1a+0.9b, 0+b.The liquid of each proportioning carries out toxicity test as stated above, checks the dead result of cotton bollworm after 48 hours, obtains the toxicity ratio table 1 of each proportioning.
The Methomyl of table 1LD50 dosage and the Toxicity Determination result of the different proportionings of CGA 183893 of LD50 dosage to cotton bollworm
According to table 1 result, take the LD50 of two single doses as the basis, form different proportionings to the toxicity test of cotton bollworm, tentatively can find out from showing, the mixture of different proportionings all has synergistic effect, their actual inhibiting rate all greater than or near 50%, the toxicity ratio is all greater than 1.Wherein the mixture actual with 0.5a+0.5b is the highest.
Therefore, the best proportioning of mixture be 50% of Methomyl LD50 value add CGA 183893 LD50 value 50%, the ratio that is converted to two single dose active ingredients then is 1: 2.6350.With reference to best proportioning result, actual in Methomyl: CGA 183893=1: 2.6 (active ingredient) is mixed, mixture preparation becomes the series concentration of certain gradient with acetone diluted, carry out Toxicity Determination, virulence regression equation, LD50 and the co-toxicity coefficient that mixture is measured also pressed the abundant method of Sun Yun and calculated co-toxicity coefficient (CTC) again.Co-toxicity coefficient CTC, computing formula is as follows: (take Methomyl as the standard medicament, its toxicity index is 100):
The LC50 of the LC50/ CGA 183893 of the toxicity index of CGA 183893 (TI)=Methomyl * 100
The LC50 of the LC50/M of the actual toxicity index (ATI) of M=Methomyl * 100
TI * the P of the theoretical toxicity index (TTI) of M=Methomyl
(Methomyl)TI * the P of+CGA 183893
(CGA 183893)
The TTI of the ATI/M of the co-toxicity coefficient of M (CTC)=M * 100
In the formula:
M is CGA 183893 and the mixture of the different proportionings of Methomyl
P
(CGA 183893)Be CGA 183893 shared ratio in mixture
P
(Methomyl)For Methomyl shared ratio in mixture sees Table 2.
Table 2 Methomyl, CGA 183893 and mixture thereof are to the Toxicity Determination result of cotton bollworm
Table 2 shows that actual in Methomyl: CGA 183893=1: 2.6 (active ingredient) is mixed, and carries out Toxicity Determination again, and co-toxicity coefficient is 151.41, and its synergistic effect is obvious.
3.1 the field experiment data are surveyed cotton bollworm, thrips, diamond-back moth
Testing program one Methomyl, CGA 183893 and mixture thereof are to the field control effectiveness test of cotton cotton bollworm
Investigation content and method:
120 insect bite leaves of every residential quarter fixed point investigation, the generation radix of record cotton cotton bollworm.Investigate the residual borer population of 120 leaves of each residential quarter fixed point respectively at 1d, 3d, 7d behind the medicine, calculate insect population decline rate and preventive effect.
Calculate drug effect by following formula:
Table 3 Methomyl, CGA 183893 and mixture thereof are to the field control effectiveness test result of cotton cotton bollworm
Interpretation of result:
Table 3 shows that complex preparation has obvious synergistic effect, and the control efficiency of high concentration treatment region obviously is better than low concentration treatment region and single dose treatment region under suitable proportioning, and the highest preventive effect can reach about 87%.It is the 3rd day control efficiency the best behind medicine, to the later stage, along with its preventive effect of volatilization of drug effect descends gradually.To crop safety, use desirable desirable control efficiency according to recommended dose.
Testing program two
Methomyl, CGA 183893 and mixture thereof are to the field control effectiveness test of eggplant thrips
Dispenser and method:
With WF-16 type knapsack hand sprayer spray medicine, shower nozzle is single fan nozzle, outlet water orifice diameter 1mm, and operating pressure is 0.2-0.4Mpa, spray amount is 0.36-0.48L/min.Conventional spraying requires uniform and delicate, leaf positive and negative even spraying.To squirt the blade face, the liquid wish is not dripped and is advisable.
Control time, number of times and method
Investigate altogether 4 times, namely at first investigate insect population radix before the medicine, the borer population remaining alive that next investigates behind the medicine 1,3,7 day calculates preventive effect.
Repeat altogether 4 times, get eggplant during investigation and push up that slightly tender leaf is some, add up the borer population alive above it, fixed point, decide strain, decide leaf investigation.
The drug effect computational methods
Borer population * 100 before decline rate (%)=(borer population after the front borer population-dispenser of dispenser)/dispenser
Preventive effect (%)=(treatment region insect population decline rate-check plot insect population decline rate)/(1-check plot insect population decline rate) * 100
Table 4 Methomyl, CGA 183893 and mixture thereof are to the field control effectiveness test result of eggplant thrips
Interpretation of result:
As shown in Table 4, Methomyl, CGA 183893 are composite under suitable dosage, not only the cotton cotton bollworm are had remarkable preventive effect, and the eggplant thrips for difficult control also has remarkable preventive effect simultaneously.The preventive effect of high concentration treatment region is apparently higher than low concentration treatment region and single dose treatment region.Behind medicine 1 day, its highest control efficiency can reach about 80%.
Testing program three
The field control effectiveness test of Methomyl, CGA 183893 and mixture wild cabbage diamond-back moth thereof
Control time and number of times
Insect population radix before the investigation medicine is investigated respectively the borer population remaining alive of 1d, 3d and 7d behind the medicine, accumulative total investigate 4 times (my god).
Investigation method
Investigate the fixedly strain of each residential quarter, investigation before the medicine is plucked first dead leaf on every side to fixing investigation strain, puts down in writing all borer populations alive, after the dispenser 1,3,7d investigates respectively the remaining borer population alive in each residential quarter.
The drug effect computational methods
Borer population * 100 before decline rate (%)=(borer population after the front borer population-dispenser of dispenser)/dispenser
Preventive effect (%)=(treatment region insect population decline rate-check plot insect population decline rate)/(1-check plot insect population decline rate) * 100
Table 5 Methomyl, CGA 183893 and mixture thereof are to the field control effectiveness test result of wild cabbage diamond-back moth
Interpretation of result:
As shown in Table 5, Methomyl, CGA 183893 are composite under suitable dosage, and the wild cabbage diamond-back moth is had remarkable preventive effect.The preventive effect of high concentration treatment region obviously is better than low concentration treatment region and single dose treatment region.Investigation in 3 days behind medicine, the highest preventive effect can reach about 77%, to crop safety.
Claims (3)
1. Pesticidal combination that contains CGA 183893 and Methomyl, it is characterized in that: the active ingredient of this Pesticidal combination is CGA 183893 and Methomyl binary built, and all the other are auxiliary element, and wherein the mass ratio of active ingredient CGA 183893 and Methomyl is 1～9: 9～1.
2. Pesticidal combination according to claim 1, it is characterized in that: CGA 183893 and the Methomyl gross weight in preparation accounts for 2%～80% of the whole quality of the pharmaceutical preparations.
3. Pesticidal combination according to claim 1 and 2, it is characterized in that: the formulation of this Pesticidal combination is missible oil, suspending agent, wetting powder, water dispersible granules, aqueous emulsion, microcapsule formulations.
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105766983B (en) * | 2012-05-16 | 2018-09-07 | 陕西汤普森生物科技有限公司 | A kind of Pesticidal combination containing CGA 183893 and anabasine |
| CN103444765A (en) * | 2012-05-31 | 2013-12-18 | 陕西汤普森生物科技有限公司 | Dicyclanil and pyrethroid-containing insecticidal composition |
| CN105265445A (en) * | 2012-06-09 | 2016-01-27 | 陕西汤普森生物科技有限公司 | Insecticide composition containing dicycla strongil |
| CN103461366B (en) * | 2012-06-09 | 2015-10-28 | 陕西汤普森生物科技有限公司 | A kind of Pesticidal combination containing CGA 183893 and carbamates |
| CN103039453A (en) * | 2012-12-26 | 2013-04-17 | 湖南海利化工股份有限公司 | Insecticidal composition containing 1-(3-fluoro-4-chlorophenyl)-2-(methylthio) ethyl ketoxime-O-(2-methyl-biphenyl-3-methyl) ether and dicyclanil |
| CN103039471B (en) * | 2012-12-26 | 2014-04-02 | 湖南化工研究院 | Insecticidal composition containing thiodicarb and dicyclanil |
| AU2017261561B2 (en) * | 2017-11-16 | 2018-08-09 | Rotam Agrochem International Company Limited | A synergistic insecticidal composition comprising methomyl and fipronil |
| CN111066785B (en) * | 2019-12-26 | 2020-11-20 | 安徽农业大学 | Application of DMNT in preparation of lepidoptera pest insecticide |
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| US4783468A (en) * | 1986-04-30 | 1988-11-08 | Ciba-Geigy Corporation | Insecticidal 5-pyrimidine carbonitriles |
| CN1257655A (en) * | 1999-12-17 | 2000-06-28 | 温沛宏 | Methomyl and cyfluthrin microemulsion as insecticide-miticide |
| CA2502427A1 (en) * | 2002-11-14 | 2004-05-27 | Novartis Ag | Combination product for controlling insect pests |
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