CN106489959B - A kind of Synergistic mite killing composition containing avermectin - Google Patents
A kind of Synergistic mite killing composition containing avermectin Download PDFInfo
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- CN106489959B CN106489959B CN201610896260.0A CN201610896260A CN106489959B CN 106489959 B CN106489959 B CN 106489959B CN 201610896260 A CN201610896260 A CN 201610896260A CN 106489959 B CN106489959 B CN 106489959B
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
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- A—HUMAN NECESSITIES
- A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
- A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
- A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
- A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
- A01N43/82—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with three ring hetero atoms
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Abstract
The invention discloses a kind of Synergistic mite killing compositions, with N- (5- tertiary butyls -1,3,4- thiadiazoles -2- bases)-N'(2,6- dichloropyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- carbonamidines（TDCA-6）It is that acceptable auxiliary element collectively constitutes in active ingredient, with pesticide with avermectin, wherein TDCA-6 and nicosulfuron weight ratio are 10:1 to 1:60.It is tested, is shown after two kinds of combination of active principles without antagonism, and there is notable synergistic effect, to crop safety by laboratory experiment and field efficacy.
Description
Technical field
The present invention relates to a kind of insecticide acaricide compositions, concretely relate to a kind of containing avermectin and the substitutions of N- tri--
The insecticide acaricide composition of 1,2,3- thiadiazoles -5- formamidine compounds, belongs to field of pesticide preparation.
Background technology
Mite class belongs to Arthropoda, Arachnoidea, Acarina, and individual is smaller.There may be all ranks in a group
The mite of section, including ovum, deutonymph, young mite and at mite.It is mostly intensive to infest fruit tree, vegetables, cotton, peanut and other crops and ornamental plant
The vacuum side of blade of object, and its breeding is rapid, high these of selfing degree all determine the more difficult prevention of mite class.On the other hand, Nong Minyou
The good single acaricide of custom continuous use miticidal effect, as a result causes acarid to generate resistance within many time and lose profit
With value.Therefore, using different role mechanism, different types of acaricide be solve evil mite be also easy to produce resistance effective way it
One.
Avermectin chemical formula C48H72O14(B1a)·C47H70O14(B1b), CAS accession number 71751-41-2, English abbreviation
Abamectin, Chinese nickname Ah going out fourth, abamectin, avermectin, avermectin, white mite are net etc..Avermectin sterling fusing point
150-155 °C, relative density 1.16 is slightly soluble in water, appearance white or pale yellow crystals powder.Presently commercially available avermectin pesticides
Be with abamectin be main insecticidal constituent (Avermectin B1a+B1b, wherein B1a are not less than 90%, 5%) B1b is no more than,
It is demarcated with the content of B1a.Avermectin solubility in common organic solvents is：Toluene 350g/L, acetone 100g/L, isopropyl
Alcohol 70g/L, chloroform 25g/L, ethyl alcohol 20g/L, methanol 19.5g/mL, hexamethylene 6g/L, kerosene 0.5g/L.Avermectin is a kind of
The agricultural or for animals sterilization that is widely used, Insecticidal and acaricidal agent.Avermectin has stomach toxicity and work of tagging to mite class and insect
With being unable to ovicidal.Mechanism of action interferes nervous physiology activity, stimulation to discharge γ-aminobutyric acid unlike general insecticide,
And γ-aminobutyric acid has inhibiting effect to the nerve conduction of arthropod.Mite class adult, nymph and insect larvae and avermectin
Occurs paralysis symptom after contact, inactive, not feeding is dead after 2~4 days.Because not causing insect rapid dehydration, so AVM hereinafter
Rhzomorph lethal effect is relatively slow.Though avermectin has direct action of contace poison to insect predator and insect parasite, because of plant
Remained on surface is few, avermectin small toxicity, therefore to the damage very little of beneficial insect.Avermectin will not be moved in soil by adsorption by soil
It is dynamic, and be decomposed by the microorganisms, thus in the environment without cumulative function, it can be as a component part of integrated control.Ah
Dimension rhzomorph common dosage forms are 1.8% missible oil (every liter contains 18 grams of active ingredient).There are many advantages of avermectin, main shortcoming
It is to mite ovum or worm's ovum poor effect, simultaneously because avermectin is used for a long time, insect pest drug resistance is caused to increase, single dose makes
With concentration through greatly increasing, therefore it is necessary to it is combined use with other efficient insecticide miticides.
Chinese patent（Application number CN2015100098343, January 9 2015 date of application, denomination of invention：Containing three nitrogen
1,2,3- thiadiazoles -5- formamidines the compound of heterocycle and synthesis）In report the artificial Xihua Univ of patent application（Inventor
The towns Wang Hui, Liu Ping, Yang Wei are clear etc.）General formula be TDCA the polysubstituted -1,2,3- thiadiazoles -5- formamidines compounds of N- and its conjunction
At method（Formula 1）.Chinese patent（Application number CN2015100237806, January 19 2015 date of application）In report patent
Apply for artificial Xihua Univ（Inventor Liu Ping, Yang Wei are clear etc.）Mutual-through type is the polysubstituted -1,2,3- thiadiazoles -5- of N- of TDCA
The novel synthesis of formamidine compound is reported that the new method uses the synthesis of target product and is first cyclized, finally upper first
The method of base obtains fine experiment effect.Chinese patent（Application number CN2015103042053, June 9 2015 date of application
Day, denomination of invention：Cyclization method synthesizes polynitrogen heterocycle thiadiazoles -5- formamidine compounds）In report the artificial Xihua of patent application
University（Clear, Liu Ping of inventor Yang Wei etc.）Mutual-through type is the polysubstituted -1,2,3- thiadiazoles -5- formamidine compounds of N- of TDCA
Novel synthesis reported that the new method is to the synthesis of target product using first upper methyl, and the method being finally cyclized, this is new
The easy preparation of synthetic method high income, catalyst, catalyst is cheap, phosphorus-containing wastewater is few, to more environment-friendly.Chinese patent
（Patent No. ZL201510277765.4, May 28 2015 date of application, 2016 Granted publication dates August 31 days, invention
Title：1,2,3- thiadiazoles -5- formamidines poly-heterocyclic compounds are as acaricidal purposes）In to report patent application artificially western
Hua Da（Inventor Yang Wei clear, Liu Ping, Zhang Yuanyuan etc.）General formula be TDCA the polysubstituted -1,2,3- thiadiazoles -5- first of N-
Amidine compound is especially used for the evil of fruit tree, vegetables, cotton, peanut and other crops and ornamental plant as acaricidal purposes
Acarid control.But polysubstituted -1,2,3- thiadiazoles -5- formamidines the compounds of N- that general formula is TDCA are to the murder by poisoning power of part adult
It is not powerful enough, need and kill the high acaricide of adult activity（Avermectin as the aforementioned etc.）Carry out interworking use.It is well known that
Insecticidal and acaricidal agent is all easy pest and develops immunity to drugs in the long-term use, to extend the service life of a new varieties, with
It is a kind of common strategy that other excellent insecticidal acaricide kinds, which carry out interworking use,.
Invention content
The main object of the present invention, by the acaricidal rational mixture of different role mechanism, is provided for the above deficiency
One kind having synergistic effect, and miticidal effect is good, safety, while can reduce the miticide composition of use cost again.
Chinese patent（Patent No. ZL201510277765.4, May 28 2015 date of application, Granted publication date
On August 31st, 2016, denomination of invention：1,2,3- thiadiazoles -5- formamidines poly-heterocyclic compounds are as acaricidal purposes）Middle report
Road general formula is N- polysubstituted -1,2, the 3- thiadiazoles -5- formamidines compounds of TDCA as acaricidal purposes, is especially used
In the control of pest mite of fruit tree, vegetables, cotton, peanut and other crops and ornamental plant.The TDCA-6 in the compound that general formula is TDCA
~TDCA-12（The detailed titles of TDCA-6~TDCA-12 and structural formula refer to Chinese Patent Application No. CN2015100098343）Tool
There is preferable acaricidal activity, considers the factors such as mite killing broad spectrum activity, toxicity, production cost, TDCA-6（Formula 2）It is numerous chemical combination
In object compare better acaricide.Therefore, in the following narrations of the present invention, general formula is mainly represented as TDCA's with TDCA-6
Polysubstituted -1,2,3- thiadiazoles -5- formamidine the compounds of N-.
What the object of the invention was realized in that：
Miticide composition of the present invention is N- (5- tertiary butyl -1,3,4- thiadiazoles -2- bases)-N&apos with Chinese;(2,6- bis-
Chloropyridine -4- bases)-N, 4- dimethyl -1,2,3- thiadiazoles -5- Jia Mis [English name is N- (5-tert-butyl-1,3,4-
thiadiazol-2-yl)-N'- (2, 6-dichloropyridin-4-yl)-N,4-dimethyl-1,2,3-
thiadiazole-5-carboxam-idine（Hereinafter referred to as TDCA-6 in the present invention）], structural formula is as shown in formula 2
Compound and avermectin be active ingredient, with pesticide in acceptable auxiliary element collectively constitute.
TDCA-6 and the permission weight ratio of avermectin are 40 in miticide composition of the present invention:1 to 1:100, preferably compare
Example is 10:1 to 1:60.
Miticide composition compound of the present invention has acaricidal purposes, is especially used for fruit tree, vegetables, cotton, peanut
The control of pest mite of equal crops and ornamental plant.The present composition is applied on crop and/or ornamental plant and is harmful to acarid life
Long region can effectively prevent evil mite.Present composition administration time can be in each growth phase in acarid, including
Ovum, deutonymph, young mite and at mite.Be mentioned below be evil mite that the present composition can be prevented some representatives, enumerate unlimited
Evil mite on following certain crops and/or ornamental plant.
As the mite class as present composition control object, can enumerate：Belong to the mite of Ying Pi sections：Japanese blood mite,
Haemaphysalis longicornis, boophilus microplus, dermacentor reticulatus, dermacentor taiwanensis, haemaphysalis flava, ixodes persulcatus etc..Belong to the mite of Eriophyidae：Tea point leaf
Save tick, tealeaves goitre mite, apple rust mite, grape leaf rust mite, tulip aceria, matrimony vine burrknot tick, pseudo- pears rust tick, Pi Shi skin goitre mites
Deng.Belong to the mite of Tyroglyphidae：Hesperidium mite, ellipse dispersion, Acarus siro, river open country fat mite, Rhizoylyphus echinopus etc..Belong to Tarsonemidae
Mite：Webster tarsonemid, Polyphagotarsonemus latus Banks, primrose herbivore mite, double leaf tarsonemid.Belong to the mite of Eupodidae：Wheat leaf pawl mite,
Chinese cabbage mite.Belong to the mite of Tetranychidae：It is panonychus citri, panonychus ulmi, mulberry Panonychus citri, Tetranychus urticae, Tetranychus cinnabarinus, purplish red short
It must mite, priet mite, Liu Shi short hairs mite, Asia beginning tetranychid, knee beginning tetranychid, northern beginning tetranychid, Lee's beginning tetranychid, Eotetranychus smithi
Deng.
Although the present composition shows the acarid of various mite sections outstanding prevention activity, to useful crop, such as
Fruit tree, vegetables, cotton, peanut and other crops and/or ornamental plant only have the damage of small degree or do not damage completely, take
Certainly in the present composition general structure concrete structure, amount of application of each compound, using useful crop object.Here it is this
Invention compound can be suitable for the basic reason of control of pest mite on crop and/or ornamental plant.
Acceptable auxiliary element in described pesticide, including at present in pesticide using, not will produce unfavorable shadow
Loud all kinds of common solvents and/or inert filler and/or surfactant and/or preservative and/or antifreezing agent and/or agglomeration resistance
Agent and/or antifoaming agent and/or cosolvent and/or the corresponding adding ingredient such as stabilizer and/or thickener, and can be according to being produced
Dosage form do corresponding selection or adjustment.
Agrochemical formulations generally comprise the miticide composition of the present invention of 0.1-99 weight %, especially 2-90 weight %.
Wettable powder（WP）Middle miticide composition is a concentration of, such as the rest part in 10-90 weight %, 100 weight % is by routinely making
Agent auxiliary element forms.In suspending agent（SC）Middle miticide composition is a concentration of, such as 1-90 weight %, preferably 5-75 weight %, and 100
Rest part in weight % is made of conventional formulation auxiliary element.In suspension emulsion（SE）Middle miticide composition is a concentration of, such as 1-
90 weight %, preferably 5-75 weight %, the rest part in 100 weight % are made of conventional formulation auxiliary element.In water dispersant
（WDG）Middle miticide composition is a concentration of, such as 1-95 weight %, preferably 10-70 weight %, and the rest part in 100 weight % is by normal
Regulation agent auxiliary element forms.The preparation of other powder types includes 1-40 weight % reactive compounds, and preferably 5-20 weight % lives
Property compound, the rest part in 100 weight % are made of conventional formulation auxiliary element.
Miticide composition of the present invention needs according to different uses or applies Huan Jing ∕ conditions, is given birth to by current conventional pesticide
TDCA-6 in the miticide composition and avermectin active ingredient and corresponding auxiliary element are that raw material is fully mixed by production mode
It closes, preparing becomes various forms of available corresponding dosage forms.Possible dosage form includes：Wettable powder, hangs water dispersant
Floating agent, aqueous emulsion, suspension emulsion, microcapsule formulations etc..Such as several typical common dosage forms and prepare can be with：
Water dispersant（WDG）Can fater disintegration in water, and can be uniformly dispersed in formation higher suspension dispersion in water
A kind of granular preparation.The present composition and auxiliary element one can be reinstated to air-flow smashing or ultra-fine grinding, system when preparation
At wettable powder, this is dry method；The present composition, auxiliary agent, adjuvant etc. are ground using water as medium in sand mill,
Suspending agent is made, then re-dry is granulated, this is wet method.
Wettable powder（WP）, i.e., solid powder preparation that in water can be evenly dispersed.It, can be according to conventional side when preparation
Formula is firstly added TDCA-6 of the present invention and the composition of avermectin, and diatomite, clay, precipitated calcium carbonate, hard charcoal is then added
The common diluent such as black or inert substance add other common auxiliary elements, as alkylnaphthalene sulfonate, alkylbenzene sulfonate,
Aliphatic alcohol sulfate, alkyl bromination ammonium, alkyl ammomium chloride, quaternary alkylphosphonium salts, alkyl polyoxyethylene base ether sulfate, lignin sulfonic acid
One or several kinds in salt, lignin, carboxymethyl cellulose, sodium carboxymethylcellulose, azone, thiophene ketone, and common stabilization
The complementary auxiliary component such as agent, foam inhibitor, anticaking agent.
Suspension emulsion（SE）I.e. the hybrid dispersions of the insoluble pesticide of water in water, one such active ingredient are in suspension
State, other active ingredients are in emulsion state.It can be by the present composition and corresponding emulsion, moistening point when being prepared when preparation
The auxiliary elements such as powder, thickener, stabilizer, antifreezing agent, pH adjusting agent, antifoaming agent, conventionally, through wet method Ultramicro-powder
It is broken to be mixed to prepare.Wherein emulsifier is alkyl phenol polyoxyethylene ether class（Agriculture breast 100#）, alkylbenzene sulfonate（Agriculture breast 500#）, benzene
Ethyl phenol polyethenoxy ether class（Agriculture breast 600#）, alkyl phenol or aralkyl phenol polyethenoxy ether formaldehyde condensation species（Nongru-700 #）
One or several kinds in.Wherein Ricinate is lignosulfonates, lignin, phosphate polyethers, carboxymethyl fibre
Tie up element, sodium carboxymethylcellulose, crown ether, alkylnaphthalene sulfonate, alkylbenzene sulfonate, aliphatic alcohol sulfate, alkyl ammonium halide, season
One or several kinds in phosphonium salt, alkyl polyoxyethylene base ether sulfate, azone, thiophene ketone；Thickener and stabilizer are polyethylene
One or several kinds in alcohol, condensed phosphate, xanthan gum, aluminum magnesium silicate etc.；Antifreezing agent be sodium chloride, urea, ammonium sulfate,
One or several kinds in ethylene glycol, glycerine etc.；PH adjusting agent be potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate,
One or several kinds in potassium carbonate etc..Common organosilicon is as antifoaming agent and foam inhibitor.
Suspending agent（SC）That is agricultural chemicals suspension agent（SC）, it is water insoluble solids pesticide or does not mix liquid pesticidal in water or oil
Dispersion.When preparation, with water or oil for decentralized medium, by TDCA-6 of the present invention and abamectin composition and auxiliary element
（Such as thickener, stabilizer, Ricinate, antifreezing agent, pH adjusting agent, antifoaming agent）Through soybean dietary fiber（Grinding）System
.Wherein Ricinate is phosphate polyethers, alkylnaphthalene sulfonate, alkylbenzene sulfonate, aliphatic alcohol sulfate, alkyl bromide
Change ammonium, alkyl ammomium chloride, crown ether, quaternary alkylphosphonium salts, alkyl polyoxyethylene base ether sulfate, lignosulfonates, lignin, carboxymethyl
One or several kinds in cellulose, sodium carboxymethylcellulose, azone, thiophene ketone；Thickener and stabilizer are polyvinyl alcohol, condensation
One or several kinds in phosphate, xanthan gum, aluminum magnesium silicate etc.；Antifreezing agent be sodium chloride, urea, ammonium sulfate, ethylene glycol,
One or several kinds in glycerine etc.；PH adjusting agent is potassium dihydrogen phosphate, dipotassium hydrogen phosphate, citric acid, sodium carbonate, potassium carbonate etc.
In one or several kinds.Common organosilicon is as antifoaming agent and foam inhibitor.
It should be noted that specific dosage form mentioned above is the representative dosage form that present composition object can be prepared, enumerate
It is not limited to these above-mentioned dosage forms.
Agrochemical formulations generally comprise the present composition object of 0.1-99 weight %, especially 0.5-95 weight %.
Wettable powder（WP）Middle activity compound concentration is, such as the rest part in 1-90 weight %, 100 weight % is by conventional formulation
Auxiliary element forms.In suspending agent（SC）Middle activity compound concentration is, such as 1-90 weight %, preferably 5-75 weight %, 100 weights
Rest part in amount % is made of conventional formulation auxiliary element.In suspension emulsion（SE）Middle activity compound concentration is, such as 1-90
Weight %, preferably 5-75 weight %, the rest part in 100 weight % are made of conventional formulation auxiliary element.In water dispersant
（WDG）Middle activity compound concentration is, such as 1-95 weight %, preferably 10-70 weight %, and the rest part in 100 weight % is by normal
Regulation agent auxiliary element forms.The preparation of other powder types includes 1-40 weight % reactive compounds, and preferably 5-20 weight % lives
Property compound, the rest part in 100 weight % are made of conventional formulation auxiliary element.
To be administered, if by appropriate formulation, dilute in a usual manner, for example, for wettable powder, water dispersant,
Suspending agent, aqueous emulsion, suspension emulsion are diluted with water.The application such as pulvis, granule, microcapsule formulations is preceding usually no longer with other inert materials
Matter dilutes.
The amount of application of the compounds of this invention changes according to external condition, and the external condition especially prevents acarid pair
As, temperature, humidity, preparation formulation.It can change in wider range, such as 0.1-500g/667m2Or more chemical combination of the present invention
Object, preferably 1-50g/667m2。
Concrete mode by the following examples is again described in further detail the above of the present invention.But it does not answer
The range that this is interpreted as to the above-mentioned theme of the present invention is only limitted to example below.The above-mentioned technological thought feelings of the present invention are not being departed from
Under condition, the various replacements or change made according to ordinary skill knowledge and customary means should all be included in the present invention's
In range.Each material composition ratio is weight % in embodiment.
Specific implementation mode：
(1), example of formulations
Embodiment 1：60% miticide composition TDCA-6 avermectin water dispersible granules（WDG）
400 grams of TDCA-6,200 grams of avermectin, 60 grams of lignin, 45 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 55 grams of polyethylene glycol, bentonite complementary are to 1000 grams（Bentonite complementary is to 1000 grams of calculated values herein
It it is 200 grams, calculation is 1000-400-200-60-45-40-55=200 gram, similarly hereinafter）, spare；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 2：50% miticide composition TDCA-10 avermectin water dispersible granules（WDG）
300 grams of TDCA-10,200 grams of avermectin, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 55 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 3：50% miticide composition TDCA-9 avermectin water dispersible granules（WDG）
300 grams of TDCA-9,200 grams of avermectin, 60 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 55 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 4：50% miticide composition TDCA-6 avermectin water dispersible granules（WDG）
200 grams of TDCA-6,300 grams of avermectin, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 30 are weighed respectively
Gram dodecyl sodium sulfate, 40 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 5：30% miticide composition TDCA-6TDCA-10 avermectin water dispersible granules（WDG）
100 grams of TDCA-6,100 grams of TDCA-10,100 grams of avermectin, 30 grams of lignin, 40 grams of acrylic acid are weighed respectively
Minor matters polymer, 30 grams of dodecyl sodium sulfates, 40 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 6：60% miticide composition TDCA-6 avermectin water dispersible granules（WDG）
Weigh respectively 571.4 grams of TDCA-6,28.6 grams of avermectin, 60 grams of lignin, 50 grams of acrylic acid minor matters polymer,
35 grams of dodecyl sodium sulfates, 25 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 7：50% miticide composition TDCA-6TDCA-13 avermectin water dispersible granules（WDG）
250 grams of TDCA-6,50 grams of TDCA-13,200 grams of avermectin, 50 grams of lignin, 50 grams of acrylic acid branches are weighed respectively
Section polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 8：30% miticide composition TDCA-6TDCA-10TDCA-13 avermectin water dispersible granules
（WDG）
Weigh respectively 100 grams of TDCA-6,100 grams of TDCA-13,50 grams of TDCA-10,50 grams of avermectin, 50 grams of lignin,
50 grams of acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 9：50% miticide composition TDCA-6TDCA-10TDCA-13 avermectin water dispersible granules
（WDG）
Weigh respectively 250 grams of TDCA-6,50 grams of TDCA-13,50 grams of TDCA-10,150 grams of avermectin, 50 grams of lignin,
50 grams of acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 60 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 10：60% miticide composition TDCA-6TDCA-10TDCA-13 avermectin water dispersible granules
（WDG）
Weigh respectively 100 grams of TDCA-6,50 grams of TDCA-13,50 grams of TDCA-10,400 grams of avermectin, 60 grams of lignin,
40 grams of acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 11：60% miticide composition TDCA-6TDCA-10TDCA-13 avermectin water dispersible granules
（WDG）
Weigh respectively 100 grams of TDCA-6,100 grams of TDCA-13,100 grams of TDCA-10,300 grams of avermectin, 60 grams it is wooden
Element, 40 grams of acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementary are standby to 1000 grams
With；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 12：60% miticide composition TDCA-6TDCA-10TDCA-13 avermectin water dispersible granules
（WDG）
Weigh respectively 150 grams of TDCA-6,150 grams of TDCA-13,150 grams of TDCA-10,150 grams of avermectin, 60 grams it is wooden
Element, 40 grams of acrylic acid minor matters polymer, 40 grams of dodecyl sodium sulfates, 50 grams of polyethylene glycol, bentonite complementary are standby to 1000 grams
With；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 13：30% miticide composition TDCA-6 avermectin water dispersible granules（WDG）
200 grams of TDCA-6,100 grams of avermectin, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 30 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 14：40% miticide composition TDCA-6 avermectin water dispersible granules（WDG）
250 grams of TDCA-6,150 grams of avermectin, 60 grams of lignin, 50 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 60 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 15：30% miticide composition TDCA-13 avermectin water dispersible granules（WDG）
200 grams of TDCA-13,100 grams of avermectin, 50 grams of lignin, 40 grams of acrylic acid minor matters polymer, 40 are weighed respectively
Gram dodecyl sodium sulfate, 40 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 16：40% miticide composition TDCA-6 avermectin wettable powders（WP）
363.6 grams of TDCA-6,36.4 grams of avermectin, 30 grams of lignosulfonates calcium, 30 grams of carboxymethyl fibres are weighed respectively
The plain sodium of dimension, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 20 grams of tetrabutylammonium bromide, kaolin complementary to 1000 grams,
It is spare；
It prepares：Each material is sequentially added in reaction kettle, stirring makes it be sufficiently mixed, and is crushed to 5~20 μm.
Embodiment 17：30% miticide composition TDCA-6 avermectin wettable powders（WP）
200 grams of TDCA-6,100 grams of avermectin, 30 grams of lignosulfonates calcium, 30 grams of carboxymethyl celluloses are weighed respectively
Sodium, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 20 grams of tetrabutylammonium bromide, kaolin complementary are standby to 1000 grams
With；
It prepares：Each material is sequentially added in reaction kettle, stirring makes it be sufficiently mixed, and is crushed to 5~20 μm.
Embodiment 18：30% miticide composition TDCA-6 avermectin wettable powders（WP）
150 grams of TDCA-6,150 grams of avermectin, 30 grams of lignosulfonates calcium, 30 grams of carboxymethyl celluloses are weighed respectively
Sodium, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 20 grams of tetrabutylammonium bromide, kaolin complementary are standby to 1000 grams
With；
It prepares：Each material is sequentially added in reaction kettle, stirring makes it be sufficiently mixed, and is crushed to 5~20 μm.
Embodiment 19：30% miticide composition TDCA-6 avermectin wettable powders（WP）
100 grams of TDCA-6,200 grams of avermectin, 30 grams of lignosulfonates calcium, 30 grams of carboxymethyl celluloses are weighed respectively
Sodium, 30 grams of aluminum magnesium silicates, 20 grams of neopelexes, 20 grams of tetrabutylammonium bromide, kaolin complementary are standby to 1000 grams
With；
It prepares：Each material is sequentially added in reaction kettle, stirring makes it be sufficiently mixed, and is crushed to 5~20 μm.
Embodiment 20：50% miticide composition TDCA-6 avermectin wettable powders（WP）
100 grams of TDCA-6,400 grams of avermectin, 40 grams of lignosulfonates calcium, 40 grams of carboxymethyl celluloses are weighed respectively
Sodium, 40 grams of aluminum magnesium silicates, 30 grams of neopelexes, 20 grams of tetrabutylammonium bromide, kaolin complementary are standby to 1000 grams
With；
It prepares：Each material is sequentially added in reaction kettle, stirring makes it be sufficiently mixed, and is crushed to 5~20 μm.
Embodiment 21：20% reactive compound（TDCA-6）Water dispersible granules（WDG）
200 grams of TDCA-6,70 grams of lignin, 60 grams of acrylic acid minor matters polymer, 50 grams of dodecyl sodium sulfonates are weighed respectively
Sodium, 80 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 22：20% avermectin water dispersible granules（WDG）
200 grams of avermectin, 70 grams of lignin, 60 grams of acrylic acid minor matters polymer, 50 grams of dodecyl sulphurs are weighed respectively
Sour sodium, 80 grams of polyethylene glycol, bentonite complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, is uniformly mixed, is then ground in sand mill, suitable quantity of water is added, is granulated,
It is drying to obtain water dispersible granules.
Embodiment 23：35% avermectin suspending agent（SC）
350 grams of avermectin, 40 grams of lignosulfonates calcium, 50 grams of sodium carboxymethylcelluloses, 30 grams of silicic acid are weighed respectively
Magnalium, 40 grams of neopelexes, 60 grams of polyethylene glycol, water complementary are spare to 1000 grams；
Each material is sequentially added in reaction kettle, just dispersion is carried out using high-speed shearing machine, is then ground in sand mill
To active ingredient grain size at 2~5 μm.
By it is following experiment it can be shown that the present invention above-mentioned miticide composition in two active ingredient TDCA-6 and Avermectin
The compounding of element can have apparent synergistic effect.
(2), biological Examples
Embodiment 24：TDCA-6 and the experiment of abamectin composition recipe determination
One, reagent agent（A represents avermectin in following reagents；B represents TDCA-6）
A agent：20% avermectin water dispersible granules（WDG）（It is prepared by the method for embodiment 22）
B agent：20% TDCA-6 water dispersible granules（WDG）（It is prepared by the method for embodiment 21）
AB1：Avermectin TDCA-6（A：B=1:1）
AB2：Avermectin TDCA-6（A：B=1:2）
AB3：Avermectin TDCA-6（A：B=1:5）
AB4：Avermectin TDCA-6（A：B=1:10）
AB5：Avermectin TDCA-6（A：B=1:20）
AB6：Avermectin TDCA-6（A：B=1:40）
AB7：Avermectin TDCA-6（A：B=1:60）
AB8：Avermectin TDCA-6（A：B=1:80）
Two, for trying insect
For examination insect using the red spider adopted in the citrus trees of field, raised for 3 generations indoors as test worm.
Three, experimental method
Experiment uses dip slide method.Each reagent tests 5 kinds of concentration（The specific concentration of each reagent refers to table 1）, each to repeat
Processing three times, repeats 120 every time, and 72 hours microscopic examination results after medicine obtain the death rate for test worm, calculate LC50With total poison
Coefficient（CTC）.
Four, computational methods
The death rate of each reagent is converted to corresponding niqueMin（y）For ordinate, and with the various concentration of various reagents
Logarithm lgx be abscissa virulence equation is obtained using least square method（y=a+blgx）Middle coefficient a, b.According to virulence side
Journey, as y=5.000（NiqueMin when i.e. the death rate is 50%）, calculate the LC of the reagent50.It is calculated using the abundant equations of Sun Yun
Go out the co-toxicity coefficient of confection（CTC）（Bibliography：Tan Genjia, wish Jianping etc., " fungicide bioassay computational methods and
Using ", Anhui agronomy notification, 1998,4（1）, 27-28）.Using the calculated CTC values of the abundant equations of Sun Yun, China is generally recognized
Being more than 150 for CTC has synergistic effect（Wherein：CTC, which is more than 200, has notable synergistic effect）, CTC is addition 50~150
Effect, it is antagonism that CTC, which is less than 50,.
Five, result and analysis
TDCA-6 and abamectin composition series match mixture to citrus red mite The Toxicity Determination result, LC50With
Co-toxicity coefficient（CTC）It is shown in Table 1, table 2.
Laboratory experiment the result shows that, TDCA-6 and abamectin composition series proportioning mixture be not aobvious to citrus red mite
Antagonism is shown, most of have certain synergistic effect, its CTC value of AB4~AB6 is all higher than 200, and wherein AB4 mixtures are total to
Malicious coefficient is maximum（CTC=216）, illustrate its synergistic effect maximum.
Table 1, TDCA-6 and avermectin match mixture to citrus red mite The Toxicity Determination result (Continued)
The death rate corresponding probit value when y represents composition series proportioning mixture various concentration in table 2, x represent concentration（C）
Logarithm lgC（That is x=lgC）.
Embodiment 25：Avermectin TDCA-6 composition for preventing and controlling citrus red mite field efficacies are tested
One, reagent agent
1,60% miticide composition TDCA-6 avermectin water dispersible granules（WDG）（According to the method system of embodiment 6
It is standby）；
2,40% miticide composition TDCA-6 avermectin wettable powders（WP）（According to the method system of embodiment 16
It is standby）；
3,20% avermectin water dispersible granules（WDG）（It is prepared according to the method for embodiment 22）；
4,20% TDCA-6 water dispersible granules（WDG）（It is prepared according to the method for embodiment 21）.
Two, experimental subjects
1, place is tested：The areas Mianyang City Nong Ke of Sichuan Province live kwan-yin village Citrus Orchard；
2, crop is tested：Sweet orange；
3, controlling object：Citrus red mite.
Three, experimental method
1, processing item：60% miticide composition TDCA-6 avermectin water dispersible granules（WDG）12000 times of dilution；
40% miticide composition TDCA-6 avermectin wettable powders（WP）8000 times of dilution；20% avermectin water-dispersible grain
Agent（WDG）4000 times of dilution；20% TDCA-6 water dispersible granules（WDG）4000 times of dilution.Blank control：Using clear water.
2, cell is arranged：Each cell seeds, the age of tree, growing way and fertilizer and water management condition are almost the same.Each cell is 3 fixed
It sets, four repetitions, totally 24 cell；And cell is arranged according to random area.
3, spraying time and method：In citrus red mite peak of occurrence period（June 25）Dispenser is primary.Using manual pressure
Contracting sprayer even spraying is degree to squirt blade.
4, control time and method：Before the application with 3 days after dispenser, 10 days, 20 days, each investigation in 30 days it is primary.Method is
Each tree wins 30 leaves at random in four orientation, and 360 are won per cell, records mite quantity living on blade, calculates mite mouthful and subtract
Move back rate and preventive effect.
Four, experimental result
60% miticide composition TDCA-6 avermectin water dispersible granules（WDG）12000 times of dilution, 40% mite killing group
Close object TDCA-6 avermectin wettable powders（WP）8000 times of processing of dilution divide citrus red mite preventive effect in 3 days after dispenser
It Wei 96.73% and 97.75%；10 days are respectively 93.01% and 93.66% to citrus red mite preventive effect after dispenser；20 days after dispenser
It is respectively 85.79% and 86.10% to citrus red mite preventive effect；30 days are respectively 80.05% He to citrus red mite preventive effect after dispenser
80.83%.The avermectin water dispersible granules of comparison medicament 20%（WDG）Dilution 4000 times, 3 days after dispenser, 10 days, 20 days, 30
It four times investigation preventive effect is respectively 94.33%, 91.42%, 82.17%, 72.06%.The TDCA-6 water dispersible granules of comparison medicament 20%
（WDG）4000 times of dilution, 3 days after dispenser, 10 days, 20 days, 30 days four times investigation preventive effects be respectively 79.88%, 75.82%,
68.23%,60.37%（Refer to table 3）.It is observed according to field experiment, does not find TDCA-6 avermectin miticide compositions to reality
It tests crop and generates poisoning phenomenon.
Claims (3)
1. miticide composition, with N- (5- tertiary butyls -1,3,4- thiadiazoles -2- bases)-N'(2,6- dichloropyridine -4- bases)-N, 4-
Dimethyl -1,2,3- thiadiazoles -5- carbonamidines and avermectin are that acceptable auxiliary element is common in active ingredient, with pesticide
Composition, wherein N- (5- tertiary butyls -1,3,4- thiadiazoles -2- bases)-N'(2,6- dichloropyridine -4- bases)-N, dimethyl -1 4-,
2,3- thiadiazoles -5- carbonamidines and avermectin weight ratio are 10:1 to 1:1.
2. miticide composition as described in claim 1, by the current conventional pesticide mode of production, prepare become it is various forms of can
For use water dispersible granules, wettable powder, suspending agent, aqueous emulsion, suspension emulsion, any one of microcapsule formulations dosage form.
3. miticide composition as described in claim 1, the control of pest mite for fruit tree, vegetables, cotton, peanut and ornamental plant.
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| CN104530040A (en) * | 2015-01-19 | 2015-04-22 | 西华大学 | Novel method for synthesizing 1,2,3-thiadiazole-5-formamidine compound |
| CN104610250A (en) * | 2015-01-09 | 2015-05-13 | 西华大学 | 1,2,3-thiadiazole-5-formamidine compound containing three N-heterocycles and synthesis |
| CN104860938A (en) * | 2015-06-08 | 2015-08-26 | 西华大学 | Multi-nitrogen heterocycle thiadiazoles-5-formamidine compound by cyclization method |
| CN104886079A (en) * | 2015-05-28 | 2015-09-09 | 西华大学 | Application of 1,2,3-thiadiazole-5-formamidine heterocyclic compound as acaricide |
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| CN104610250A (en) * | 2015-01-09 | 2015-05-13 | 西华大学 | 1,2,3-thiadiazole-5-formamidine compound containing three N-heterocycles and synthesis |
| CN104530040A (en) * | 2015-01-19 | 2015-04-22 | 西华大学 | Novel method for synthesizing 1,2,3-thiadiazole-5-formamidine compound |
| CN104886079A (en) * | 2015-05-28 | 2015-09-09 | 西华大学 | Application of 1,2,3-thiadiazole-5-formamidine heterocyclic compound as acaricide |
| CN104860938A (en) * | 2015-06-08 | 2015-08-26 | 西华大学 | Multi-nitrogen heterocycle thiadiazoles-5-formamidine compound by cyclization method |
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