CN104642373B - A kind of containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin - Google Patents
A kind of containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin Download PDFInfo
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- CN104642373B CN104642373B CN201510061001.1A CN201510061001A CN104642373B CN 104642373 B CN104642373 B CN 104642373B CN 201510061001 A CN201510061001 A CN 201510061001A CN 104642373 B CN104642373 B CN 104642373B
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Abstract
The invention discloses a kind of containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin, containing chlorine fluorine cyanogen insect amide 15% 23%, gamma cyhalothrin 3% 15%, surplus is auxiliary agent and oils filler, and percent concentration therein is weight percentage.The dosage form of this Pesticidal combination preferably dispersibles oil-suspending agent, preparation technology is: grind and " rear emulsion dispersion " combined techniques, the creamy oil phase of class will be prepared as by gamma cyhalothrin, the chlorine fluorine cyanogen insect amide that addition Conventional milling methods prepares dispersibles in oil-suspending agent, makes its emulsion dispersion uniformly form by high shear dispersion machine；This insecticides to dispersible oil-suspending agent excellent to being easily generated the lepidoptera pest preventive effect such as drug-fast diamondback moth, there is crop affinity good, quick-acting has concurrently with lasting effect, the feature such as when producing and use environmental stimulus is low, can be used for the resistance management of diamondback moth.
Description
Technical field
The invention belongs to pesticide field, be specifically related to a kind of containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin
And dispersible the preparation method of oil-suspending agent.
Technical background
Chlorine fluorine cyanogen insect amide (test code number ZJ4042) is Zhejiang Research Institute of Chemical Industry, Ltd.'s (country's south pesticide wound
Base, Zhejiang, center processed) autonomous innovation development, the phthalic diamides insecticide of cyano-containing, obtain country's invention specially
Profit, Zhejiang Hetian Chemical Co., Ltd. is the industry development base in base, Zhejiang, pesticides discovery center, country south.This former medicine
Low toxicity, to rabbit eyes and no skin irritation, without three mutagenicities and genotoxicity, is that one is the safest, efficiently,
The environment-friendly pesticide of low toxicity.
Show according to the Toxicity Determination result of open source information report, its insecticidal spectrum, insecticidal bioactivity, and insecticidal action side
Formula, all suitable with novel pesticide fipronil bisamide to lepidopterous larvae poisoning symptom etc., thus it is speculated that its mechanism of action is similar to fluorine worm
Bisamide class.
Gamma cyhalothrin is efficient, the pyrethroid Insecticidal and acaricidal agent of wide spectrum, fast-acting type, to tag and stomach toxicity work
With for main, without systemic action, generally its that insect knocks down activity is the highest, drug effect is rapid, it is adaptable to Semen arachidis hypogaeae, Semen sojae atricolor, cotton
Flower, fruit tree, vegetable, in the various crop such as Folium Camelliae sinensis on the preventing and treating of many Species of Lepidopterous Insect Pests, it is possible to be used for preventing and treating multiple earth's surface and
Public health insect.
Gamma cyhalothrin former medicine fusing point about 49 DEG C, in a lot of organic solvents, dissolubility is the best, generally its processing agent
Type is cream.
Dispersibling oil-suspending agent (oil-based suspension concentrate, OD) is FAO (Food and Agriculture Organization of the United Nation) in recent years
(FAO) that releases is efficient, the green dosage form of environment-friendly type, and it is with the oils of environment-friendly type as medium, is suspended by stable effective ingredients
Liquid preparation in oil；Suitably it is processed into the pesticide activity component dispersibling oil-suspending agent, the most at least possesses two features:
One is that former medicine fusing point wants high (being advisable for more than 60 degree), and two is that former medicine is the most insoluble in oil based media；Otherwise it produces and adds
Work difficulty will be the biggest；Generally its processing technique is ground exactly, is i.e. ground to form necessarily by material by the abrasive media in sand mill
The granule of fineness, and make it be dispersed in oil based media by the peptizaiton of surfactant.
This dosage form, owing to containing a large amount of plant oils, for comparing water, it is much better to the affinity of crop and target, therefore should
Dosage form not only increases the medicament efficiency of transmission to target organisms, and to environment with the most friendly.Comparatively speaking,
Then there is bigger environmental issue in cream and wettable powder, the former is because employing a large amount of organic solvent disagreeableness to environment, after
Then there is serious dust problem in person, therefore, dispersibles the dosage form that oil-suspending agent is a kind of very high-efficiency environment friendly, its use time with
Use after water dilution allotment uniformly.
Diamondback moth is a kind of global important pests taking food brassicaceous vegetable of causing harm specially, often causes sternly to agricultural production
The loss of weight.Since from nineteen fifty-three reported first, it develops immunity to drugs, successively in China Shanghai, Guangdong, Hainan, Shandong etc. is many
Individual area is found that diamondback moth is to organophosphor, carbamate, pyrethroid and benzoyl group phenylurea class insect growth regulator, IGR etc.
More than 50 kind of insecticide all creates Drug resistance；When diamondback moth is caused harm serious, even if strengthening dosage, still can not efficiently control it
Cause harm；This makes safety and environmental protection and efficient diamondback moth pesticide control the most rare, and many times peasant has to use high poison
The even pesticide of severe toxicity class goes preventing and treating.On the one hand this can strengthen peasant's user exposure when high poison highly toxic pesticide uses,
Endanger healthy；On the other hand the high poison thus brought, highly toxic pesticide residue problem carrys out hidden trouble also to food seat belt.
Summary of the invention
The purpose of the present invention: one is to provide a kind of efficient for the important pests diamondback moth on the crops such as vegetable and be not likely to produce Drug resistance
Novel environment friendly insecticide；Two is to dispersible the preparation of oil-suspending agent for the dosage form of this insecticide composition to provide one and newly add
Work technique.
First purpose of the present invention is achieved through the following technical solutions:
A kind of containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin, it is characterised in that: described insecticide composition
Thing contains chlorine fluorine cyanogen insect amide 15%-23%, gamma cyhalothrin 3%-15%, and surplus is auxiliary agent and oils filler, therein
Percent concentration is weight percentage.
Further, chlorine fluorine cyanogen insect amide content is preferably 15%-18%, gamma cyhalothrin 7%-10%；Surplus is auxiliary agent
With oils filler.
Described oils filler is vegetable oil or methylated vegetable oil, and oils filler is selected from soybean oil, Semen Maydis oil, Oleum Ricini, dish
One or several in seed oil, olive oil, methyl oleate, methyl hexadecanoate, esterification soybean oil, esterification Oleum Brassicae campestris,
Account for the 50%-70% of Pesticidal combination weight ratio.
Described auxiliary agent includes emulsifying agent, dispersant, penetrating agent, thickening agent or PH regulator.
The dosage form of described insecticides preferably dispersibles oil-suspending agent.
Above-mentioned dispersible in oil-suspending agent, in addition to containing active component and vegetable oil or methylated vegetable oil, live possibly together with surface
Property agent and thickening agent, add PH regulator etc. if desired.
Surfactant can serve as emulsifying agent, dispersant or penetrating agent, can be nonionic and anionic, also
It can be two or more compound use.Described emulsifying agent is selected from polyoxyethylene ether oleoyl ricinoleate, castor oil polyoxyethylene
Ether, polyoxyethylene ether glycerine ester, polyethylene glycol monooleate, EO-PO (polyoxyethylene polyoxypropylene) graft block copolymerization
Thing, styrenated phenol polyoxyethylene ether phosphate triethanolamine salt, described dispersant is selected from macromolecule oiliness polycarboxylate.Above-mentioned
Surfactant accounts for the 10%-30% of Pesticidal combination weight ratio.
The thickening agent of indication of the present invention is organic modified bentonite, gas-phase silica, polyamide wax etc..PH regulator is organic amine
Deng.
Second object of the present invention is achieved through the following technical solutions:
The preparation method dispersibling oil-suspending agent of a kind of insecticides, it is characterised in that described insecticides contains
Chlorine fluorine cyanogen insect amide 15%-23%, gamma cyhalothrin 3%-15%, surplus is auxiliary agent and oils filler, percentage ratio therein
Concentration is weight percentage；The described preparation method dispersibling oil-suspending agent is as follows: first by chlorine fluorine cyanogen insect amide and auxiliary agent, oils
Filling material grinding becomes to dispersible oil-suspending agent；Again gamma cyhalothrin and plant oil, emulsifying agent are prepared as the creamy oil of class
Phase；Finally by this oil phase add chlorine fluorine cyanogen insect amide dispersible in oil-suspending agent, make it disperse by high-shear emulsifying dispersion machine
Uniformly, prepare chlorine fluorine cyanogen insect amide and gamma cyhalothrin dispersibles oil-suspending agent.
The new processing technique of composite preparation in the present invention, is different from traditional single mill method.It should be understood that efficient chlorine
Flucythrinate fusing point is low, easily heats up due to machinery equipment during grinding, especially produces equipment heating bigger, prepared by single grinding
Technique easily makes it melted and sedimentation occurs to assemble, thus cause the processing technique of routine cannot normally prepare chlorine fluorine cyanogen insect amide with
Gamma cyhalothrin complex dispersible oil-suspending agent, and described new preparation process reasonably avoiding gamma cyhalothrin
Process of lapping so that the oil-suspending agent that dispersibles of chlorine fluorine cyanogen insect amide and gamma cyhalothrin is successfully prepared.
In the above-mentioned composition of the present invention, chlorine fluorine cyanogen insect amide is in stomach poison function mode, and owing to being noval chemical compound, it is made
It is still not clear by mechanism, but its structurally and functionally mode, and insect is all analogous to fipronil bisamide by the dead worm symptom after medicine,
Therefore speculate that it is that calcium ion discharges accelerator, even if insect excessively discharges calcium ion, thus cause body calcium deficiency thus paralysis and
Extremely.Gamma cyhalothrin is pyrethroid efficient pesticides, model of action to tag and stomach toxicity, its mechanism of action
For nervous system aixs cylinder position conduction depressant drug, make insect the most dead by destroying neural conduction.
The present invention utilizes the Action mechanism that chlorine fluorine cyanogen insect amide is brand-new and the stomach poison function showed, and has diamondback moth larvae
Preferably insecticidal effect and the lasting period；Utilize gamma cyhalothrin quickly to tag and stomach poison function, make insect larva anti-by medicine
Faster should there is certain osmosis additionally, due to gamma cyhalothrin on blade face, the useful effect agent of compound drug can be improved
Amount and rain wash resistance.
Chlorine fluorine cyanogen insect amide is compounding with gamma cyhalothrin produces synergistic function, it is possible to overcome two kinds of single doses to use
Deficiency, on the one hand chlorine fluorine cyanogen insect amide single dose is used alone, and responding time is relatively slow；Diamondback moth is to efficiently the most at present
Lambda-cyhalothrin Drug resistance is increasing, and two kinds of composite reagents use, and the synergism between them greatly strengthen drug effect, makes
The improvement of the compositions of the present invention Lepidoptera class pest such as diamondback moth to producing resistance also has an effect of uniqueness, and due to
Drug effect improves, it is also possible to reduce both dosages, and the edible safety risk reducing vegetable is also had benifit.
Through it is demonstrated experimentally that the insecticides of the present invention has extraordinary parasite killing to the vegetable diamondback moth developed immunity to drugs
Effect, is a kind of ideal Pesticidal combination.
The process equipment of present composition preparation and the processing technique do not stated clearly be disclose known.
Detailed description of the invention:
The present invention in order to illustrate, but is not limited to these examples with the following example that is embodied as.In all formula, percentage ratio is all attached most importance to
Amount ratio.
One, the preparation of oil-suspending agent is dispersibled
By chlorine fluorine cyanogen insect amide and auxiliary agent, oils weighs, and loads sand mill after homogenizing, and the particle diameter of sand milling to preparation is at 10 microns
Hereinafter, thus obtain homogeneous dispersibling oil-suspending agent finished product；Again by gamma cyhalothrin and emulsifying agent, oils mixes, and stirs
Mix and be prepared as oil phase to clarification；Finally this oil phase addition chlorine fluorine cyanogen insect amide is dispersibled in oil-suspending agent, use high-shear emulsifying
Dispersion machine is sheared uniformly, and obtain described compositions dispersibles oil-suspending agent.
Formulation Example one: chlorine fluorine cyanogen insect amide 15%, gamma cyhalothrin 10%, polyoxyethylene ether oleoyl ricinoleate 15%,
Colophonium grafting EO-PO block copolymer 2%, macromolecule modified oil base polycarboxylate 2%, modified alta-mud 1.5%, soybean oil
Supply 100%.
Formulation Example two: chlorine fluorine cyanogen insect amide 17%, gamma cyhalothrin 8%, polyoxyethylene ether oleoyl ricinoleate 15%,
Colophonium grafting EO-PO block copolymer 2%, macromolecule modified oil base polycarboxylate 2%, gas-phase silica 1%, bentone
Soil 1%, soybean oil supplies 100%.
Formulation Example three: chlorine fluorine cyanogen insect amide 19%, gamma cyhalothrin 6%, polyoxyethylene ether glycerine ester 10%, Colophonium
Grafting EO-PO block copolymer 3%, castor oil polyoxyethylene ether 5%, macromolecule modified oil base polycarboxylate 2%, gas phase
White carbon 1%, modified alta-mud 1%, methyl oleate supplies 100%.
Formulation Example four: chlorine fluorine cyanogen insect amide 21%, gamma cyhalothrin 4%, polyethylene glycol monooleate 10%, polyoxy second
Alkene ether glycerine ester 10%, macromolecule modified oil base polycarboxylate 2%, gas-phase silica 1%, modified alta-mud 0.5%, beautiful
Miyou supplies 100%.
Two, effect experiment method
(1) chlorine fluorine cyanogen insect amide and the compositions of gamma cyhalothrin are to diamondback moth indoor biometrics experimental technique
Use cabbage leaves infusion process.Main for fresh cabbage leaves muscle is removed, is cut into about 3cm × 5cm leaf dish with shears, will
2～3 leaf dish are dipped in medicinal liquid 10 seconds, after ventilation is dried naturally, are placed in diameter 10cm culture dish, and every ware connects
3 mid-term in age diamondback moth larvae 20, lid absorbent paper, add a cover, labelling, temperature (26 ± 2) DEG C, relative humidity 70%,
Intensity of illumination 2000lx, Light To Dark Ratio is the indoor of 14h:10h.Test sets 3 repetitions, compares with clear water.24h、72h
" Invest, Then Investigate " diamondback moth larvae death condition, to touch polypide with brush pen during investigation, examination worm is motionless or can not normally creep as dead worm mark
Accurate.
Note: the 96% chlorine former medicine of fluorine cyanogen insect amide used is provided by Zhejiang Provincial Chemical Engineering Research Inst pesticides discovery；For examination diamondback moth 3
Instar larvae picks up from the same Caulis et Folium Brassicae capitatae ground that Drug resistance is more serious.
(2) test statistics
Add up each borer population alives processed and total borer population, calculating mortality rate (Abbott ' s formula).
Carry out data analysis statistical by " DPS data handling system " V6.50 professional version, obtain regression straight line, LC50.Use grandson
Yun Peifa (Sun etc. 1960) calculates toxicity index and co-toxicity coefficient.
Toxicity index × the A of theoretical mixed toxicity index (TTI)=A content (%) in mixed
Toxicity index × the B of+B content (%) in mixed
(3) effect experiment result
With the insecticides of the present invention and chlorine fluorine cyanogen insect amide, gamma cyhalothrin single dose carries out contrast test, to pickles
Co-toxicity coefficient and the test of pesticide effectiveness data of moth are as shown in table 1.
Table 1: chlorine fluorine cyanogen insect amide combines diamondback moth co-toxicity coefficient measurement result (following chlorine fluorine cyanogen insect amide with gamma cyhalothrin
Replacing with A, gamma cyhalothrin B replaces)
| Insecticide | LC50(mg/L) | Actual measurement toxicity index | Theoretical toxicity index | Co-toxicity coefficient CTC |
| A | 5.86 | 2455.63 | / | / |
| B | 143.9 | 100 | / | / |
| A:B=12:13 | 5.24 | 2746.18 | 1230.702 | 223.139 |
| A:B=15:10 | 4.17 | 3450.84 | 1513.378 | 228.022 |
| A:B=18:7 | 3.24 | 4441.36 | 1796.054 | 247.284 |
| A:B=20:5 | 3.21 | 4482.87 | 1984.504 | 225.894 |
| A:B=23:2 | 3.83 | 3757.18 | 2267.180 | 165.720 |
The evaluation of complex preparation insecticidal effect, is mainly judged by calculating co-toxicity coefficient (Cotoxicity Cotteient, CTC).If
Co-toxicity coefficient CTC is more than 120, shows there is potentiation；If less than 80, being shown to be antagonism；Close to 100, it is shown to be
Summation action.
From the point of view of above-mentioned indoor biometrics experimental result, the combination of above-mentioned chlorine fluorine cyanogen insect amide and gamma cyhalothrin to 3 age pickles
Moth is respectively provided with preferable potentiation (CTC value is all higher than 120).
After described compositions is prepared as dispersibling oil-suspending agent, with 20% chlorine fluorine cyanogen insect amide aqueous suspension agent, 5% efficient cyhalothrin
Emulsifiable concentrate has carried out field medicine effect test contrast for rice leaf roller, and data are as follows:
Table 2: chlorine fluorine cyanogen insect amide and gamma cyhalothrin dispersible oil-suspending agent to rice leaf roller control in field effect
From the point of view of control in field effect, chlorine fluorine cyanogen insect amide has preferable preventive effect with the combination of gamma cyhalothrin to diamondback moth,
After 14 days, mortality rate all can reach more than 83%.Drug effect all has raising in various degree compared with single dose, especially with chlorine fluorine cyanogen insect amide
15%-18%, during gamma cyhalothrin 7%-10%, potentiation is the most prominent, hence it is evident that be better than chlorine fluorine cyanogen insect amide and efficient chlorine
Flucythrinate single dose, the preventive effect after 14 days is all more than 90%.
From the point of view of above-mentioned experimental result, chlorine fluorine cyanogen insect amide can have quick-acting and lasting effect concurrently with the combination of gamma cyhalothrin,
And it is capable of preferable efficiency-cost ratio, and it is a kind of preferably insecticide composition, the improvement of antagonism diamondback moth is a preferably selection.
Claims (6)
1. a containing chlorine fluorine cyanogen insect amide and the insecticides of gamma cyhalothrin, it is characterized in that: described insecticides contains chlorine fluorine cyanogen insect amide 15%-23%, gamma cyhalothrin 3%-15%, surplus is auxiliary agent and oils filler, and percent concentration therein is weight percentage.
Insecticides the most according to claim 1, it is characterised in that described insecticides contains chlorine fluorine cyanogen insect amide 15%-18%, gamma cyhalothrin 7%-10%, surplus is auxiliary agent and oils filler.
Insecticides the most according to claim 1, it is characterized in that: described oils filler is vegetable oil or methylated vegetable oil, oils filler is selected from one or several in soybean oil, Semen Maydis oil, Oleum Ricini, Oleum Brassicae campestris, olive oil, methyl oleate, methyl hexadecanoate, esterification soybean oil, esterification Oleum Brassicae campestris.
Insecticides the most according to claim 1, it is characterised in that described auxiliary agent includes emulsifying agent, dispersant, penetrating agent, thickening agent or PH regulator.
Insecticides the most according to claim 1, it is characterised in that the dosage form of described insecticides is for dispersibling oil-suspending agent.
6. the preparation method dispersibling oil-suspending agent of an insecticides, it is characterized in that, described insecticides contains chlorine fluorine cyanogen insect amide 15%-23%, gamma cyhalothrin 3%-15%, surplus is auxiliary agent and oils filler, and percent concentration therein is weight percentage；The described preparation method dispersibling oil-suspending agent is as follows: first become to dispersible oil-suspending agent with auxiliary agent, oils filling material grinding by chlorine fluorine cyanogen insect amide；Again gamma cyhalothrin and plant oil, emulsifying agent are prepared as the creamy oil phase of class；What this oil phase finally added chlorine fluorine cyanogen insect amide dispersibles in oil-suspending agent, makes it be uniformly dispersed by high-shear emulsifying dispersion machine, and prepare chlorine fluorine cyanogen insect amide and gamma cyhalothrin dispersibles oil-suspending agent.
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| CN106857690A (en) * | 2015-12-11 | 2017-06-20 | 黄少安 | A kind of insecticide |
| CN106259497A (en) * | 2016-08-15 | 2017-01-04 | 卞佳林 | A kind of Synergistic type method for producing insecticide |
| CN112741085B (en) * | 2020-12-30 | 2022-04-12 | 中国农业科学院植物保护研究所 | Trichoderma conidium oil suspending agent and application thereof |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007122264A2 (en) * | 2006-04-26 | 2007-11-01 | Basf Se | Composition comprising a glucan or a glucan derivative and a pesticide and methods for improving plant health |
| CN102613183A (en) * | 2012-03-07 | 2012-08-01 | 中化蓝天集团有限公司 | Insecticide |
| CN102626077A (en) * | 2012-04-01 | 2012-08-08 | 广西田园生化股份有限公司 | Ultra-low-volume liquid containing flubendiamide |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2007122264A2 (en) * | 2006-04-26 | 2007-11-01 | Basf Se | Composition comprising a glucan or a glucan derivative and a pesticide and methods for improving plant health |
| CN102613183A (en) * | 2012-03-07 | 2012-08-01 | 中化蓝天集团有限公司 | Insecticide |
| CN102626077A (en) * | 2012-04-01 | 2012-08-08 | 广西田园生化股份有限公司 | Ultra-low-volume liquid containing flubendiamide |
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Effective date of registration: 20221014 Address after: 343000 Tengfei Branch Road, Salt Chemical Industrial City, Xingan County, Ji'an City, Jiangxi Province Patentee after: Jiangxi Hetian Technology Co.,Ltd. Address before: 310018 Plot M-18-5-4, Hangzhou Economic and Technological Development Zone, Hangzhou, Zhejiang Patentee before: ZHEJIANG HETIAN CHEMICAL Co.,Ltd. Patentee before: LIANYUNGANG HETIAN CHEMICAL Co.,Ltd. |