CN103798282A - Insecticide composition containing pirimiphos-methyl and micro-capsule suspending agent thereof - Google Patents
Insecticide composition containing pirimiphos-methyl and micro-capsule suspending agent thereof Download PDFInfo
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Abstract
The invention provides an insecticide composition containing pirimiphos-methyl and a micro-capsule suspending agent thereof. The insecticide composition comprises a component A and a component B, wherein the component A is the pirimiphos-methyl; the component B is selected from one of pyriproxyfen, chlorbenzuron, diflubenzuron and triflumuron; the mass ratio of the component A to the component B ranges from (100:1)-(2:1), most preferably 50:1; the highest cotoxicity coefficient is 224.1 and the insecticidal efficacy is optimal. The invention provides the insecticide composition containing pirimiphos-methyl and the micro-capsule suspending agent thereof; the organic phosphorus type efficient, low-toxin and wide-spectrum pirimiphos-methyl and insect growth regulators (juvenile hormone types) including the low-toxin compounds of the pyriproxyfen, the chlorbenzuron, the diflubenzuron and the triflumuron are compounded so as to effectively delay the drug resistance caused by sanitary insect pests such as cockroaches, mosquitoes and flies; the effects of killing imagoes and larvae can also be realized.
Description
Technical field
The present invention relates to a kind of composite composition pesticide and pesticide processing field, be specifically related to a kind of pirimiphos-methyl and the composite Pesticidal combination of insect growth regulator, IGR and its microcapsule suspending agent of containing, be applied to hygienic insecticide field.
Background technology
Sanitary insect pest refers to that those can produce directly or indirectly harm to human health, affects all arthropodss of people's normal life, comprises two classes: Insecta and arachnids Acari.Mosquito, fly, cockroach (blattaria), termite, flea, bedbug all belong to Insecta.The harassing and wrecking and parasitic of sucking blood of the main harm of sanitary insect pest, and the sanitary insect pest of some kind is the communication media of some infectious disease of the mankind, very large to people's health hazard, once outburst easily forms epidemic situation.
Pirimiphos-methyl (Pirimiphos-methyl).Chemical name: O-O-dimethyl-O-(2-diethylin-6-methylpyrimidine-4-yl)-phosphorothionate.
Pirimiphos-methyl is a kind of wide spectrum, quick-acting organophosphorus insecticides and the miticide of ICI company exploitation in 1974, belongs to anticholinesterase.Have and tag and fumigation action.Its mechanism of action is to suppress the activity of cholinesterase in organism, and it is without interior absorption.Various pests to coleoptera, diptera, Lepidoptera, Homoptera and mite class is effective, and it not only can prevent and treat grain storage insect and domestic hygiene insect effectively.The WHO of Ta Shi World Health Organization recommendation is at one of agricultural chemicals hygienic insecticide of sanitary insect pest control.The editor of WHO tropical disease control administration, " chemical prevention and control method of important medium biology " middle promotion pirimiphos-methyl of publishing are used for the control of the sanitary insect pests such as mosquito, fly, mouse flea, Pulex irritans, bedbug, cockroach and mite.
The fusing point of pirimiphos-methyl industrial goods is 15～18 ℃; When distillation, decompose; Vapour pressure 2mpa (20 ℃); Relative density 1.17 (20 ℃); Solvability is 9.9 (PH5.2) in water, 8.6 (PH7.3), and 9.3 (PH9.3) (being mg/l30 ℃ entirely), can be dissolved in most of organic solution as ethanol, acetone, alkyl halide; Can be by strong acid and basic hydrolysis, half life period 7.5d～35d (between pH value scope 5.8～8.5, the most stable when PH7), under daylight, the half life period of its aqueous solution is 1d; Flash-point >46 ℃; The common formulation in market has: pulvis, missible oil, aerosol, aqueous emulsion.
Pyriproxyfen, diflubenzuron, triflumuron, the young urea that goes out etc. belong to insect growth regulator, IGR, can be good at that interference insect is grown normally, casted off a skin, delayed development, thereby cause normally casting off a skin, grow and dead.
Pyriproxyfen (pyriproxyfen) chemical name: 4-phenoxy phenyl (RS)-2-(2-pyridine radicals oxygen) propyl ether, physicochemical property: fusing point: 45-47 ℃, density: 1.32, condition of storage: 0-6 ℃, sterling is crystallization.Vapour pressure 0.29 × 10-3Pa (20 ℃), relative density 1.23 (20 ℃).Solvability is: dimethylbenzene 50g, hexane 40g.Pyriproxyfen is the insect growth regulator, IGR of upsetting insect growth, has interior suction transfer activity, low toxicity, and the lasting period is long, to crop safety, and to fish low toxicity, the feature little to eco-environmental impact.This product has good control efficiency to the sanitary insect pest such as fly, mosquito.There is mosquito, fly larvae pupation and the emergence effect of inhibition.Mosquito, fly larva contact this medicament, substantially, all in death in pupa time, can not sprout wings.This medicament lasting period reached about 1 month, and easy to use, and free from extraneous odour is good kill mosquito, fly medicine.Common preparation has: 0.5% granule, 10% missible oil.
230 ℃～232 ℃ of diflubenzuron (Diflubenzuron) fusing points.Solvability: water 0.08mg/L (pH5.5,200C), acetone 6.5g/L (20 ℃), dimethyl formamide 104g/L (25 ℃), moderate is dissolved in polar organic solvent.Insecticidal mechanism: Main Function is the chitin synthesis that suppresses insect cuticle, the internal secretion such as fat-body, corporal allata and body of gland is had again to damage destruction simultaneously, thus hinder the smooth molt metamorphosis of insect.After insect takes food, cause accumulation property poisoning, owing to lacking chitin, larva can not form new epidermis, and the difficulty of casting off a skin pupates to be obstructed; Adult is difficult to sprout wings, lay eggs; Ovum can not normal development, the larva epidermis of hatching lacks hardness and death.To other biological safety in people and animals and environment, belong to low toxicity public nuisance-free agricultural chemicals.
Triflumuron (Triflumuron) is a kind of insect growth regulator, IGR.It is mainly stomach poison function to insect, has certain action of contace poison, but without systemic action, has good ovicidal action.Triflumuron belongs to low toxic pesticide, suppresses insect chitin synthetic, makes casting off a skin of insect pupate to be obstructed, and activity slows down, and takes food minimizing, even dead.Mainly, take stomach toxicity as main, have certain action of contace poison concurrently, to most animals and humans nonhazardous effects, and can be decomposed by Institute of Micro-biology, because it is efficient, low toxicity and wide spectrum, become the principal item of current conditioning agent class agricultural chemicals.
The young urea (chlorbenzuron) that goes out belongs to insect growth regulator, IGR.By suppressing the activity of insect cuticle chitin synthetase and urine nucleosides coenzyme, thereby suppress that insect chitin is synthetic causes insect normally not cast off a skin and dead.Use in larval phase, the new epidermis of insect is formed and be obstructed, delayed development, or lack hardness, can not normally cast off a skin and cause death or form lopsided pupa death.Almost harmless to the hymenopteran such as beneficial insect and honeybee and Forest birds.Larvae to control lavatory fly maggot, stagnant water gulf also has special efficacy.
Some active ingredients of the frequent use of public health insecticide are all mainly pyrethroids, due to long-term use, the sanitary insect pest colony that is is for a long time under the selection pressure in this insecticides, the gene of target biology is undergone mutation, susceptibility to insecticide constantly declines, cause pesticide resistance to produce, the difficulty of control continues to increase.Pirimiphos-methyl is as important sanitary insect pest control medicine, and the sanitary insect pest that especially chrysanthemum ester class has been produced to resistance demonstrates higher biologically active.Pirimiphos-methyl, to the micro-poison of mammal, to environment non-target organism safety, is a kind of good sanitary insect pest insecticide of high-efficiency low-toxicity, and its benefit is invisible.Pyriproxyfen, diflubenzuron, the young urea that goes out etc. are a kind of insect growth regulator, IGRs, the people in environment for use and livestock safety, and the mechanism of action of himself is that the sanitary insect pest such as fly, mosquito is had to mosquito, fly larvae pupation and the emergence effect of inhibition simultaneously.If mosquito, fly larva contact this pyriproxyfen, substantially all in death in pupa time, and can not sprout wings into adult.With the exception of this, insect growth regulator, IGR antagonism insect (to organic phosphor, carbamate, organochlorine, pyrethroid insectide) activity does not have difference, can not be subject to the impact of resistance.
In the prior art, publication number is disclosed a kind of public health insecticide of CN101715783A patent publications and preparation method thereof, and it is a kind of complex composition of pirimiphos-methyl and gamma cyhalothrin chrysanthemum ester.It is the effervescent tablet take 2.5% gamma cyhalothrin and 6% pirimiphos-methyl as active ingredient.Gamma cyhalothrin has individual shortcoming as a kind of hygienic insecticide, be exactly that the former medicine of pyrethroid is general all with the sensitization to human body, especially gamma cyhalothrin has very strong sensitization to the skin of human body, cause itch, redness, the comfort level affect its use concerning operator and livestock time.Publication number is that 102657160A discloses " insecticide pirimiphos-methyl micro-capsule suspension and preparation method ", and its product is single dose product, and effect composition is single compound, and capsule material uses shitosan-aliphatic poly ester material.Be that CN101848642A discloses " pesticide compositions " pesticide compositions is provided at publication number, comprise the former medicine complex preparation containing pirimiphos-methyl and a kind of plants essential oil and chrysanthemum ester class.
At " Agriculture in Hunan science " 2002(4) in " synergistic effect and the application thereof to corn weevil of pirimiphos-methyl and malathion " literary composition, a kind of complex composition of pirimiphos-methyl and malathion is disclosed, be mainly used in the control of grain pest, its controlling object is corn weevil, red flour beetle, is mainly the occupation mode adopting fumigation of grain.Malathion belongs to a kind of agricultural chemicals of organic phosphates, and former medicine itself has garlic odour taste, and industrial goods itself have strong impulse nature and flavor road, uses so be generally used in the granary of sealing, can not serve as human settlement's health medication.
In " pesticide research and the application " time: 2011 issues: the 6th phase; Author: the people such as Tu Ximao deliver in " research that complex coacervation is prepared pirimiphos-methyl micro-capsule suspension " literary composition, first be the single dose preparation of a pirimiphos-methyl, adopt complex coacervation to prepare microcapsule suspending agent, one-tenth capsule material is the natural wall materials such as gelatin, gum Arabic, but this class natural polymer becomes capsule casing material that capsule material forms to be difficult to realize the function of controlling active ingredient in release microcapsule, because complex coacervation is more difficult control in actual production process, therefore in business-like micro-capsule, seldom have the method for employing, preparation is unitary agent.In " pesticide research and the application " time: 2010 issues: the 4th phase; Author: the people such as Li Yan deliver in " development of 20% pirimiphos-methyl microcapsule suspending agent " literary composition, adopts situ aggregation method to prepare the pirimiphos-methyl microcapsules that Lauxite is wall material, is a kind of single dose about pirimiphos-methyl.
Summary of the invention
In order to address the above problem, the object of the present invention is to provide the Pesticidal combination and the microcapsule suspending agent thereof that contain pirimiphos-methyl, the organic phosphates pirimiphos-methyl that adopts efficient, low toxicity, wide spectrum with carry out composite as the low toxicity compounds pyriproxyfen of insect growth regulator, IGR (protecting young parahormone class), the young urea that goes out, diflubenzuron, triflumuron, can effectively delay the sanitary insect pest such as blattaria, mosquitos and flies and develop immunity to drugs, can reach again the double effect of controlling of adult and larva.
Technical solution of the present invention is as follows:
The invention provides the Pesticidal combination that contains pirimiphos-methyl, described Pesticidal combination comprises component A and B component, described component A is pirimiphos-methyl, the one that described B component is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron, the mass ratio of described component A and B component is 100:1～2:1.
The Pesticidal combination that contains pirimiphos-methyl of the present invention, preferably the mass ratio of described component A and B component is 50:1～20:1, synergistic effect is especially obvious.
The Pesticidal combination that contains pirimiphos-methyl of the present invention, most preferably the mass ratio of described component A and B component is 50:1, now co-toxicity coefficient 224.1, synergistic effect is the most obvious.
The Pesticidal combination that contains pirimiphos-methyl of the present invention, preferably, the mass ratio of described pirimiphos-methyl and pyriproxyfen is 50:1～20:1, and mosquitos and flies is had to good control efficiency.
The Pesticidal combination that contains pirimiphos-methyl of the present invention, further preferably, the optimum quality ratio of described pirimiphos-methyl and pyriproxyfen is 50:1, now co-toxicity coefficient is 224.1.
The present invention also provides the microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination described in a kind of comprising, comprises the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, the one that described active component B is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron.
The invention provides the microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination described in a kind of comprising, preferably, comprise the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, the one that described active component B is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron.
The invention provides the microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination described in a kind of comprising, most preferably, comprise the component of following proportioning, by percentage to the quality:
Described active components A is pirimiphos-methyl, the one that described active component B is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described solvent is selected from the one in methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters cocoa butter, turpentine-based vegetable oil and fatty acid ester; Most preferably methyl esters soybean oil, methyl esters palm oil, turpentine-based vegetable oil.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described stabilizing agent is selected from epoxidized soybean oil, 2, the one in 6-toluene di-tert-butyl phenol (BHT), butylated hydroxy anisole (BHA), triphenyl phosphite and potassium dihydrogen phosphate.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described attractant is selected from the one in 1-octyne-3-alcohol, fatty glyceride, glyceride lactate, lactic acid lactone and amino acid.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described cyst material is selected from carbamide resin, melamine resin, polyurethane, polyesteramide, the one in fatty polyamide resin, polyvinyl acetate resin and polystyrene resin.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described dispersant is selected from the one in aromatic sulphonate, acrylic acid and acrylic ester copolymers, formaldehyde condensation products sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt class, styrene alkyl polyoxyethylene ether phosphate and sodium lignin sulfonate.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described emulsifier is selected from the one of anhydrous sorbitol laurate, polyoxyethylene laurel ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene monopalmitate and Emulsifier EL-60.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described antifreeze is selected from the one in ethylene glycol, propane diols, glycerine, isopropyl alcohol and urea, preferably propane diols.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described preservative is selected from the one in Sodium Benzoate and KF88.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described viscosity-controlling agent is selected from the one in xanthans, carragheen, gelatin, aluminium-magnesium silicate and bentonite, preferably xanthans.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described PH acid-base modifier is selected from the one in glacial acetic acid, citric acid, ammoniacal liquor, triethanolamine and sodium hydroxide.
The microcapsule suspending agent that contains pirimiphos-methyl Pesticidal combination of the present invention, preferably, described water is deionized water or distilled water.
The application's Pesticidal combination itself has the insecticidal effect of good sanitary insect pest, said composition is after microencapsulation simultaneously, be prepared into after microcapsule suspending agent, in the time of residual spray, there is good lasting effect, the drug effect data of embodiment all illustrate this point, and these are well more a lot of than the effect of common microcapsule suspending agent.
The invention provides by above-mentioned composition and prepare and be applicable to the microcapsule suspending agent formulation form that agricultural chemicals uses, above-mentioned dosage formulation can also be prepared by known method, and the present composition also can be prepared as granule GR, wetting powder WP, suspension emulsion SE, microemulsion ME, aqueous emulsion EW or water dispersible granules WDG etc.
The invention provides a kind of for preventing and treating the hygienic insecticide of sanitary insect pest mosquito, fly, it is the complex preparation that contains pirimiphos-methyl, its active ingredient comprises active components A and active component B, wherein active components A is pirimiphos-methyl, and active component B is any one in following insect growth regulator, IGR: pyriproxyfen, diflubenzuron, young urea, triflumuron go out;
Embodiment of the present invention microcapsule suspending agent comprises the component of following weight proportion: be prepared into microcapsule suspending agent, be made up of active component, stabilizing agent, attractant, emulsifier, one-tenth capsule material, dispersant, antifreeze, preservative, water; Basic components is as follows:
| Component | Mass percent |
| Active components A | 0.1%～60% |
| Active component B | 0.01%～10% |
| Solvent | 0.5%～5% |
| Stabilizing agent | 0.1%～3% |
| Attractant | 0.01%～1% |
| Emulsifier | 1%～3% |
| Become capsule material | 3%～10% |
| Dispersant | 1%～8% |
| Antifreeze | 1%～5% |
| Preservative | 0.1%～0.3% |
| Thickener | 0.01%～0.3% |
| Water | Complement to～100% |
Active components A in formula is pirimiphos-methyl, and former medicine purity is greater than more than 95% high-purity former medicine, does not almost make us unjoyful stink;
Active component B in formula is: wipe out the flies and mosquitoes, diflubenzuron, the one of going out in young urea and triflumuron;
Solvent in formula does not use the dimethylbenzene that uses in traditional pesticidal preparations, aromatic solvent naphtha, polar solvent etc., but has used solvent methylated vegetable oil (as: methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters coconut wet goods plant resource methyl esters oil), turpentine-based vegetable oil, fatty acid ester of environmental protection etc.;
In the present invention, having added stabilizing agent, is mainly the special physico-chemical character because of the former medicine of pirimiphos-methyl, and pirimiphos-methyl is the same with other organophosphorus insecticide, and at memory period, also objective reality active ingredient is held labile problem.And then cause the decline of properties of product, cause product not reach pesticide supplying effect.As everyone knows, the factor that affects organic phosphor phosphate pesticide stability is mainly the purity of former medicine and the stability of chemical constitution.The stabilizing agent Main Function of this formula screening is: 1. the physics and the chemical stability that keep and strengthen the former medicine of pirimiphos-methyl; 2. be to prevent gentle decomposition of separating the former medicine of pirimiphos-methyl.Mainly from following material, select one: epoxidized soybean oil, 2,6-toluene di-tert-butyl phenol (BHT), butylated hydroxy anisole (BHA), triphenyl phosphite, potassium dihydrogen phosphate;
Attractant: the insecticide that the present invention relates to a kind of sanitary insect pest, so add therein some attractants, its action principle is the smell information of sex attractant and the secretion of simulation domestic animal, so that the attracting action to mosquitos and flies after dispenser is better, attract the probability of licking of the contact of mosquito and fly, thereby improve insect killing efficiency.From following component, select: 1-octyne-3-alcohol, fatty glyceride, glyceride lactate, lactic acid lactone, amino acid etc.;
Cyst material in formula is carbamide resin, melamine resin, polyurethane, polyesteramide, fatty polyamide resin, polyvinyl acetate resin, polystyrene resin;
Dispersant in formula is selected the one in aromatic sulphonate, acrylic acid and acrylic ester copolymers, formaldehyde condensation products sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt class, styrene alkyl polyoxyethylene ether phosphate, sodium lignin sulfonate;
Emulsifier in formula is selected the one of anhydrous sorbitol laurate, polyoxyethylene laurel ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene monopalmitate, Emulsifier EL-60;
The antifreeze using in formula is ethylene glycol, propane diols, glycerine, isopropyl alcohol, urea, preferably propane diols;
Preservative in formula: the one in Sodium Benzoate, KF88;
Viscosity-controlling agent in formula is selected from xanthans, carragheen, gelatin, aluminium-magnesium silicate, bentonite, our preferred xanthans;
The PH acid-base modifier using in formula is the one in glacial acetic acid, citric acid, ammoniacal liquor, triethanolamine, sodium hydroxide;
The water adopting in this production technology: be deionized water or distilled water.
The technique effect that the present invention is useful:
The Pesticidal combination that contains pirimiphos-methyl provided by the invention and microcapsule suspending agent thereof adopt that organic phosphates is efficient, low toxicity, the pirimiphos-methyl of wide spectrum and low toxicity compounds pyriproxyfen, the young urea that goes out, diflubenzuron, the triflumuron of insect growth regulator, IGR (protecting young parahormone class) composite, can effectively delay the sanitary insect pest such as blattaria, mosquitos and flies and develop immunity to drugs, can reach again the double effect of controlling of adult and larva.
The present invention has overcome the deficiency containing single-activity component insecticide, and the blattaria developing immunity to drugs because of long-term prescription, mosquito, fly, termite, flea etc. are had to the anti-effect of holding concurrently, and reduces formulation rate simultaneously, reduces drug cost and the pollution to environment.
The microcapsule suspending agent tool of the Pesticidal combination that contains pirimiphos-methyl provided by the invention has the following advantages: because control to active ingredient pirimiphos-methyl discharges thereby has the longer lasting period, reduce the number of times of dispenser by (1) after this Pesticidal combination after microencapsulation; (2) active ingredient is wrapped in cyst wall and has improved safety, makes preparation reduce toxic grade; (3) active component B belongs to insect growth regulator, IGR steroids former medicine, slowly discharges and contributes to extend emergence time and the larvae pupation of controlling mosquito, fly after being wrapped in capsule casing material in environment; (4) some unhappy smells and skin irritation material is effectively reduced; (5) reduce due to the steam loss that brings active ingredient of volatilizing.
Embodiment
In order to make object of the present invention, technical scheme and advantage clearer, the present invention describes with following specific embodiment, but the present invention is limited to absolutely not these examples.The following stated is only the good embodiment of the present invention, only for explaining the present invention, can not therefore be interpreted as the restriction to the scope of the claims of the present invention.It should be pointed out that all any modifications of making within the spirit and principles in the present invention, be equal to alternative and improvement etc., within all should being included in protection scope of the present invention.
Preparation of the present invention is by the processing method of existing formulations of pesticide comparative maturity, by the common method such as pirimiphos-methyl and pyriproxyfen, auxiliary agent, make the preparations such as glue bait formulation, wetting powder, aqueous emulsion, suspension emulsion, missible oil, microemulsion, microcapsule suspending agent, ultra low volume spraying agent in the ratio in embodiment.The preferred microcapsule suspending agent of the present invention is inventive embodiments.Reagent used is commercial.Apart from outside specified otherwise, all percentage is weight ratio in these embodiments
Embodiment 1 laboratory determination of activity report:
Experiment purpose:
With the monochromatic Ability of Culex Pipiens Larvae of the laboratory rearing mark target of making a living, measure the mixed agent of each single dose and pirimiphos-methyl and pyriproxyfen to the virulence of monochromatic Ability of Culex Pipiens Larvae, calculate composite mixture co-toxicity coefficient, determine synergistic effect power.
Assay method:
Measure the larva eradicative rate of each processing, calculate composite mixture co-toxicity coefficient.The comprehensive index of correlation of reason everywhere, the proportioning that selective advance effect is strong analyzed.By mosquito larvae being immersed in to the 24h lethality obtaining in different liquids, obtain LC50.
1, test material: test tools made: dilute liquid medicine with 50ml volumetric flask several, some, adjustable pipette, some, the beaker of all size, selects the suction pipe number that larva uses and props up.Insecticide: select the preparation of pure medicine or high concentration, take acetone as solvent, first medicament is configured to 1% mother liquor control Refrigerator store for subsequent use.When experiment, be configured to again 0.1% mother liquor, when configuration needs concentration, all press active ingredient and calculate; For testing worm: monochromatic culex, 4 instar larvaes.
2. method of testing: immersion method, select 4 instar larvaes to put into small beaker, 20 every glass, then supply water yield 50ml.Each large beaker adds 200ml dechlorination running water.On every beaker, answer labeled test medicine name and concentration value.Then, the liquid that is configured in the variable concentrations in volumetric flask, therefrom draw respectively 1ml with pipette, liquid splashes in water, then stirs evenly with glass bar.At this moment larva in measuring cup is all poured in beaker together with 50ml water, add up to into the 250ml aqueous solution.Each concentration has 3 repetitions at least, and control group is set, and splashes into equally blank solvent liquid.After 24h, check death toll.While checking the dead quantity of larva, available tip tweezers are touched lose favour head and afterbody respiratory siphon gently, if slow in reacting and can not be floating to level, or the larva of the thick seemingly-dead dress of language, calculate in the lump in death toll.Error Pass Test requirement, available Abbott common recognition corrected mortality calculate LD50.
Carry out statistical analysis with DPS data processing software, calculate the LC50(half lethal concentration of each medicament) and reagent agent EC50(half-maximal effect concentration), then press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).
When CTC≤80, composition performance, for antagonism, is worked as 80<CTC<120, and composition performance is for summation action, and when CTC >=120, composition performance is synergistic effect.
Actual measurement toxicity index (ATI)=(standard medicament EC50/ reagent agent EC50) × 100;
The percentage composition of B in percentage composition+B medicament toxicity index × mixture of A in theoretical toxicity index (TTI)=A medicament toxicity index × mixture;
Co-toxicity coefficient (CTC)=[the theoretical toxicity index of mixture actual measurement toxicity index (ATI)/mixture (TTI)] × 100;
The Toxicity Determination result of different disposal to monochromatic Ability of Culex Pipiens Larvae
Four, discussion of results
In the scope of the weight proportion 100:1～2:1 of pirimiphos-methyl and pyriproxyfen, between the obvious weight proportion 50:1～20:1 of synergistic effect, select methyl Midinyanglin and the monochromatic Ability of Culex Pipiens Larvae of pyriproxyfen complex preparation (50:1) to carry out toxicity test, its co-toxicity coefficient is 224.1, and synergistic effect is especially obvious.
Embodiment 2 laboratory determination of activity reports:
Control mosquito, fly indoor pharmacodynamic test; Test target: Culex pipiens pallens, the 3rd day～female insect of not sucking blood for the 5th day after sprouting wings; Housefly, the adult of 3rd～4 days after sprouting wings, female, hero half and half; Test method: with reference to GB T13917.10-2009, cage test; Experiment is processed: preparation is diluted to equal working concentration.
Result of the test shows: the single dose missible oil of control sample 9,10 is not so good as 1～8 composite sample for the drug effect of mosquito, fly in knocking down property, but the composite sample of pirimiphos-methyl and pyriproxyfen is fine to the down effect of mosquitos and flies, and also has good lethality rate.
Data result can be found out: at pirimiphos-methyl and pyriproxyfen is composite that mosquitos and flies 24h lethality rate preventive effect is all reached more than 95%, kill mosquitos and flies respond well.Meet 24h mosquitos and flies lethality rate and reach 100%, simultaneously aspect knocking down property KT50min reasonable weight proportion between 50:1～20:1.
This combines composite preparation, the sanitary insect pest such as mosquito, fly is had to reasonable control efficiency, there is good rate of knockdown to have again good lethality rate simultaneously, put and exempt to have significant synergies at control sanitary insect pest, can reduce the usage amount of preparation, cost-saving, delay the drug-fast generation of sanitary insect pest simultaneously.
Embodiment 1:
Active components A pirimiphos-methyl 6g, the active component B young urea 0.06g that goes out joins in solvent 2g methyl esters soybean oil and stirs, after add again stabilizing agent epoxidized soybean oil 0.2g, emulsifier fatty alcohol-polyoxyethylene ether 1g, attractant 1-octyne-3-alcohol 0.02%, adds encystation monomer toluene di-isocyanate(TDI) 2g to stir and obtains oil phase; By dispersant polymerization of carboxylic acid sodium salt class 2g and antifreeze ethylene glycol 5%, preservative KF88 0.1%, thickener xanthans 0.3%g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 40 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, keeps temperature 6 hours, and adopting interfacial polymerization to obtain carbamide resin is 6.06% pirimiphos-methyl of the capsule material young urea microcapsule suspending agent (active components A: active component B=100:1) that goes out.
Embodiment 2:
Active components A pirimiphos-methyl 24g, active component B pyriproxyfen 0.3g joins in solvent 4g rosinweed oil and stirs, after add again stabilizing agent triphenyl phosphite 0.3g, emulsifier polyoxyethylene castor oil 1g, attractant glyceride lactate 0.1g, adds encystation monomer toluene di-isocyanate(TDI) 4g to stir and obtains oil phase; By dispersant acrylic acid and acrylic ester copolymers 5g and antifreeze propane diols 5%, preservative sodium benzoate 0.1%, thickener xanthans 0.2g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 45 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, keeps temperature 4 hours, adopts interfacial polymerization to obtain the 24.3% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=80:1) that carbamide resin is capsule material.
Embodiment 3:
Active components A pirimiphos-methyl 30g, active component B pyriproxyfen 0.6g joins in solvent 2.5g rosinweed oil and stirs, after add again emulsifier polyoxyethylene bay ether 2g, attractant fatty glyceride 0.1g stirs and obtains oil phase; Antifreeze glycerine 3g, stabilizing agent potassium dihydrogen phosphate 0.2g, encystation performed polymer formaldehyde-urea performed polymer 10g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 60 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, add in batches watery hydrochloric acid to regulate pH=2.5 that polycondensation reaction occurs, keep temperature 4 hours, again dispersant sodium lignin sulfonate 6g, thickener carragheen 0.2%g, preservative sodium benzoate 0.2% are added and stirred, change example and adopt situ aggregation method to obtain the 30.6% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=50:1) that Lauxite is capsule material.
Embodiment 4:
Active components A pirimiphos-methyl 60g, active component B diflubenzuron 2g joins in solvent 2g methyl esters palm oil and stirs, after add again stabilizing agent BHA0.3g, emulsifier anhydrous sorbitol laurate 1g, attractant lactic acid lactone 0.1, add into capsule material 4,4-methyl diphenylene diisocyanate 6g stirs and obtains oil phase; By dispersant copolymer-maleic anhydride sodium salt 2g and antifreeze ethylene glycol 1g, preservative KF88 0.1%, thickener xanthans 0.01g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 40 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, keeps temperature 8 hours, adopts interfacial polymerization to obtain the 62% pirimiphos-methyl diflubenzuron microcapsule suspending agent (active components A: active component B=30:1) that carbamide resin is capsule material.
Embodiment 5:
Active components A pirimiphos-methyl 40g, active component B pyriproxyfen 2g joins in solvent 4g methyl esters cocoa butter and stirs, after add again stabilizing agent BHT0.1g, emulsifier polyoxyethylene monopalmitate 2g, attractant amino acid 0.1g stirs and obtains oil phase; By dispersant lignosulfonates 4g and antifreeze glycerine 3g, preservative KF88 0.2g, become capsule material polyvinyl acetate emulsion 4g, thickener xanthans 0.05g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 60 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, keep temperature 4 hours, adopt suspension polymerization to obtain the 42% pirimiphos-methyl pyriproxyfen microcapsule suspending agent (active components A: active component B=20:1) that polyvinyl acetate resin is capsule material.
Embodiment 6:
Active components A pirimiphos-methyl 10g, active component B triflumuron 1g joins in solvent 1g corn methyl esters oil and stirs, after add again emulsifier fatty alcohol-polyoxyethylene ether 1g, attractant 1-octyne-3-alcohol 0.1g stirs and obtains oil phase; Antifreeze propane diols 5g, stabilizing agent potassium dihydrogen phosphate 0.1g, encystation performed polymer melamine-formaldehyde prepolymer 5g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 45 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, add in batches watery hydrochloric acid to regulate pH=3.5 that polycondensation reaction occurs, keep temperature 6 hours, again dispersant sodium lignin sulfonate 3g, thickener xanthans 0.3%g, preservative sodium benzoate 0.2% are added and stirred, change example and adopt situ aggregation method to obtain the 11% pirimiphos-methyl triflumuron microcapsule suspending agent (active components A: active component B=10:1) that melamine resin is capsule material.
Embodiment 7:
Active components A pirimiphos-methyl 0.5g, active component B diflubenzuron 0.1g joins in solvent 10g methyl esters cocoa butter and stirs, after add again stabilizing agent epoxidized soybean oil 0.2g, emulsifier anhydrous sorbitol laurate 2g, attractant amino acid 0.1g stirs and obtains oil phase; By dispersant according to carboxylate 3g and antifreeze ethylene glycol 5g, preservative KF88 0.2g, triethanolamine 0.1g, thickener xanthans 0.3g, encystation monomer styrene emulsion 0.4g be added to the water (water complements to 100g) stir and obtain water; By oil, water preheat to 35 ℃, then oil phase poured into water and opened emulsify at a high speed, by the time stable emulsion, keeps temperature 8 hours, adopts suspension polymerization to obtain the 0.6% pirimiphos-methyl diflubenzuron microcapsule suspending agent (active components A: active component B=5:1) that polystyrene resin is capsule material.
The residual spray drug effect result of 1～7 pair of housefly of embodiment, Culex pipiens pallens:
Assay method: carry out according to GB13917.1-92.By sample by a certain percentage with after distilled water diluting, recommend routinely effective dose to be coated on breadboard face, the breadboard face of dispenser is at room temperature deposited, and with dispenser after the 1st day, 7 days, 30 days, employing forces contact method, makes to try worm contact plate face 30min with the contactor that forces that is parallel to plate face, then examination worm is moved to clean raising in cylinder, clean cage and raises, observed and recorded Culex pipiens pallens 24h lethality, housefly 24h lethality.Test in triplicate, is carried out blank test, gets rid of error.By Abbott formula calculation correction lethality.
Drug effect result: the active component A pirimiphos-methyl active component B microcapsule suspending agent that this embodiment 1～7 prepares is applied to the control of Culex pipiens pallens, housefly.Embodiment medicament is coated on plate face by recommendation concentration ratio thin up, recommended density 1～the 2g(a.i of residual spray control housefly, Culex pipiens pallens pirimiphos-methyl preparation active ingredient)/m2,1 day, 7 days and 30 days control efficiency to sanitary insect pest after statistics medicine.Result is as follows:
As can be seen from the table, pass through composite pyriproxyfen, diflubenzuron, triflumuron etc. by pirimiphos-methyl, sanitary insect pest is obtained to good synergistic effect, can effectively fall and delay the low resistance that insect produces control medicament, can effectively extend the control time by the complex preparation after microencapsulation, obtain good residual spray effect.Aspect the quick-acting of killing to mosquitos and flies and lasting effect significantly better than single dose.
The composite microcapsule suspending agent of combination of the present invention and the 30% pirimiphos-methyl microcapsule suspending agent single dose contrast contrasting, be not difficult to find out that composition after composite to the control efficiency of mosquitos and flies more, same time (7d, 30d) after residual spray, control efficiency is all better than microcapsule suspending agent single dose.By the composite desinsection pedigree that expanded, delay the pesticide resistance of sanitary insect pest, improve the lasting effect of residual spray.
Claims (10)
1. contain the Pesticidal combination of pirimiphos-methyl, it is characterized in that, described Pesticidal combination comprises component A and B component, described component A is pirimiphos-methyl, the one that described B component is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron, the mass ratio of described component A and B component is 100:1～2:1.
2. the Pesticidal combination that contains according to claim 1 pirimiphos-methyl, is characterized in that, the mass ratio of described component A and B component is 50:1～20:1.
3. the Pesticidal combination that contains according to claim 1 pirimiphos-methyl, is characterized in that, the mass ratio of described component A and B component is 50:1.
4. the hygienic biocide composition that contains according to claim 1 pirimiphos-methyl, is characterized in that, the mass ratio of described pirimiphos-methyl and pyriproxyfen is 50:1～20:1.
5. the hygienic biocide composition that contains according to claim 4 pirimiphos-methyl, is characterized in that, the mass ratio of described pirimiphos-methyl and pyriproxyfen is 50:1.
6. a microcapsule suspending agent, is characterized in that, comprises the Pesticidal combination that contains pirimiphos-methyl described in claim 1-3 any one, and the component of described microcapsule suspending agent proportioning is as follows, by percentage to the quality:
Described active components A is pirimiphos-methyl, the one that described active component B is selected from pyriproxyfen, goes out in young urea, diflubenzuron and triflumuron.
7. contain according to claim 6 the microcapsule suspending agent of pirimiphos-methyl Pesticidal combination, it is characterized in that, described stabilizing agent is selected from epoxidized soybean oil, 2, the one in 6-toluene di-tert-butyl phenol, butylated hydroxy anisole, triphenyl phosphite and potassium dihydrogen phosphate.
8. the microcapsule suspending agent that contains according to claim 6 pirimiphos-methyl Pesticidal combination, is characterized in that, described attractant is selected from the one in 1-octyne-3-alcohol, fatty glyceride, glyceride lactate, lactic acid lactone and amino acid.
9. contain according to claim 6 the microcapsule suspending agent of pirimiphos-methyl Pesticidal combination, it is characterized in that, described cyst material is selected from carbamide resin, melamine resin, polyurethane, polyesteramide, the one in fatty polyamide resin, polyvinyl acetate resin and polystyrene resin.
10. contain according to claim 6 the microcapsule suspending agent of pirimiphos-methyl Pesticidal combination, it is characterized in that, described solvent is selected from the one in methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters cocoa butter, turpentine-based vegetable oil and fatty acid ester;
Described dispersant is selected from the one in aromatic sulphonate, acrylic acid and acrylic ester copolymers, formaldehyde condensation products sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt class, styrene alkyl polyoxyethylene ether phosphate and sodium lignin sulfonate;
Described emulsifier is selected from the one of anhydrous sorbitol laurate, polyoxyethylene laurel ether, fatty alcohol-polyoxyethylene ether, polyoxyethylene monopalmitate and Emulsifier EL-60;
Described antifreeze is selected from the one in ethylene glycol, propane diols, glycerine, isopropyl alcohol and urea, preferably propane diols;
Described preservative is selected from the one in Sodium Benzoate and KF88;
Described viscosity-controlling agent is selected from the one in xanthans, carragheen, gelatin, aluminium-magnesium silicate and bentonite, preferably xanthans;
Described water is deionized water or distilled water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106538591A (en) * | 2016-10-31 | 2017-03-29 | 陕西先农生物科技有限公司 | Pesticidal combination containing pirimiphos-methyl and preparation method thereof |
| CN107087633A (en) * | 2017-05-08 | 2017-08-25 | 南通功成精细化工有限公司 | A kind of hygienic biocide composition containing pirimiphos-methyl and its application |
| CN111345313A (en) * | 2018-12-24 | 2020-06-30 | 江苏扬农化工股份有限公司 | Fly-killing composition for controlling fly breeding place and application thereof |
| CN114600875A (en) * | 2022-02-22 | 2022-06-10 | 武汉市拜乐卫生科技有限公司 | Fly killing bait and preparation method thereof |
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| WO2006008109A2 (en) * | 2004-07-20 | 2006-01-26 | Bayer Cropscience Ag | Insecticidal agents based on selected insecticides and safeners |
| CN1739351A (en) * | 1996-04-29 | 2006-03-01 | 诺瓦蒂斯公司 | Pesticide composition |
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Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1739351A (en) * | 1996-04-29 | 2006-03-01 | 诺瓦蒂斯公司 | Pesticide composition |
| WO2006008109A2 (en) * | 2004-07-20 | 2006-01-26 | Bayer Cropscience Ag | Insecticidal agents based on selected insecticides and safeners |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106538591A (en) * | 2016-10-31 | 2017-03-29 | 陕西先农生物科技有限公司 | Pesticidal combination containing pirimiphos-methyl and preparation method thereof |
| CN107087633A (en) * | 2017-05-08 | 2017-08-25 | 南通功成精细化工有限公司 | A kind of hygienic biocide composition containing pirimiphos-methyl and its application |
| CN111345313A (en) * | 2018-12-24 | 2020-06-30 | 江苏扬农化工股份有限公司 | Fly-killing composition for controlling fly breeding place and application thereof |
| CN114600875A (en) * | 2022-02-22 | 2022-06-10 | 武汉市拜乐卫生科技有限公司 | Fly killing bait and preparation method thereof |
| CN114600875B (en) * | 2022-02-22 | 2023-12-15 | 武汉市拜乐卫生科技有限公司 | Fly killing bait and preparation method thereof |
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Address after: 226006, Jiangsu, Nantong Province Economic and Technological Development Zone, West revitalization of the South and east of Jiangdong carbon Co-patentee after: U.N. Nantong Pesticide Formulation Development Center Patentee after: Nantong liannong Jiatian crop Technology Co. Ltd. Address before: 226006 No. 3, Zhenxing West Road, Nantong economic and Technological Development Zone, Jiangsu Co-patentee before: U.N. Nantong Pesticide Formulation Development Center Patentee before: Nantong Liannong Pesticide Formulation R&D Co., Ltd. |
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Granted publication date: 20150923 Termination date: 20210307 |