CN102113483A - Acaricidal composition containing chlorfenapyr and spirodiclofen - Google Patents
Acaricidal composition containing chlorfenapyr and spirodiclofen Download PDFInfo
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- CN102113483A CN102113483A CN2010100015723A CN201010001572A CN102113483A CN 102113483 A CN102113483 A CN 102113483A CN 2010100015723 A CN2010100015723 A CN 2010100015723A CN 201010001572 A CN201010001572 A CN 201010001572A CN 102113483 A CN102113483 A CN 102113483A
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- chlorfenapyr
- spiral shell
- mite ester
- shell mite
- miticide composition
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Abstract
The invention discloses an acaricidal composition containing chlorfenapyr and spirodiclofen and a preparation method and application thereof. The acaricidal composition is characterized by containing the chlorfenapyr, the spirodiclofen and other aids, wherein the weight ratio of the chlorfenapyr to the spirodiclofen is (0.1-30):(0.1-30). The acaricidal composition can be applied to the prevention and control of various harmful acarids. The composition is safe and environmentally-friendly, and has low cost and good effects. Indoor virulence tests and field tests prove that: the composition has obvious synergy. Moreover, the compounding of the chlorfenapyr and the spirodiclofen is not reported in China and foreign countries, so the acaricidal composition is provided.
Description
Technical field
The invention belongs to field of agrochemicals, it is acaricidal composite to relate to agricultural insecticide, is the acaricidal composite of main active and application thereof with spiral shell mite ester and chlorfenapyr especially.
Background technology
Using chemical agent is the most effectively means of control plant insect evil mite.But long-term use single chemical insecticide continuously high dose, cause residual, the environmental pollution of medicament and the problems such as development that anti-resistanc pest does harm to mite easily.Reasonably chemical insecticide is composite or be mixed and have the expansion insecticidal spectrum, improve control efficiency, prolong the optimum period for applying fertilizer, reduce dosage, reduce poisoning, reduce residual, delay insect evil mite drug resistance and positive characteristics such as drug-fast generation and development, insecticidal/acaricidal agent is composite or to be mixed be one of the effective method the most that addresses the above problem.Exploitation new product insecticide price is constantly soaring, and by contrast, exploitation is efficient with research, low toxicity, low-residual composite be mixed have small investment, the lead time is short and be subjected to domestic and international attention, strengthens the development dynamics one after another.
Spiral shell mite ester (English spirodiclofen):
Chemical molecular formula C
12H
24Cl
2O
4, the mechanism of action is destroyed the energy metabolism activity of acarid for suppressing the lipogenesis in the evil mite body, finally kills harmful mite.The characteristics of control are to kill that mite broad spectrum activity, ovum children are held concurrently and killed, the lasting period is long, toxicity is low, safety is good and other miticides do not have cross resistance, and shortcoming is speed of action slow (drug effect peak be behind the medicine about 7 days), and is undesirable to one-tenth mite effect.By China's pesticide toxicity grading criteria, spiral shell mite ester belongs to the low toxicity miticide.Be widely used in various mite class controls, as Panonychus citri, cotton spider mites, the Tetranychus cinnabarinus of Tetranychidae apple, citrus, Tarsonemidae (the many tarsonemids of side), Eriophyidae (thorn apple rust mite, grape rust mite), Tenuipalpidae (grape brevipalpus).But the spiral shell mite ester of Xiao Shouing is a unitary agent in the market, and this unitary agent in use easily produces resistance, and the defective that the preventive effect cost rises day by day, speed of action is slower is arranged.
Chlorfenapyr:
Have another name called capillary, external title is named and is eliminated, and belongs to aryl and adjoins and coughs up compounds, is by the chemical constitution transformation that contains the pyrrole ring natural antibiotics is successfully developed, and absorption is very strong in it, and the while is used non-resistant mutually with other drug.Insect is had stronger stomach poison function and certain action of contace poison, its mechanism of action uniqueness, the lasting period is long, and the evil of the various pests on fruit tree, vegetables, cotton, legume crop mite is had preventive effect preferably.Toxicity to the person poultry toxicity is lower, is the efficient pesticide-miticide of quite being paid close attention at present.
Summary of the invention
The objective of the invention is at above-mentioned variety of issue,, thereby provide a kind of miticide composition of preventing and treating various crop mite class disease for the pesticide resistance, the expansion that overcome and delay existing agricultural chemicals are killed the mite spectrum, strengthen drug effect, reduced drug cost.Two kinds of compounds that the present invention relates to composite do not have report at present as yet.
A further object of the invention provides the purposes of this miticide composition.
Measure of the present invention realizes by following measures.
A kind of miticide composition, it contains spiral shell mite ester and chlorfenapyr, and wherein the weight ratio of spiral shell mite ester and chlorfenapyr is 0.1~30: 0.1~30.
Described miticide composition, wherein the more excellent weight ratio of spiral shell mite ester and chlorfenapyr is 0.5~30: 0.5~30.
Described miticide composition, wherein to accumulate the weight ratio of shared preparation be 1~60% to two kinds of active principles of spiral shell mite ester and chlorfenapyr.
Described miticide composition, spiral shell mite ester and chlorfenapyr and auxiliary agent, carrier etc. are processed into any one formulation that allows on the agricultural chemicals.
Described miticide composition is characterized in that the formulation that can be processed into is suspending agent, aqueous emulsion, microemulsion, wetting powder, water dispersible granules and microcapsule formulations etc.
Described miticide composition is used to prevent and treat the multiple mite class on tetranychus viennensis, apple tetranychus, panonychus ulmi, Tetranychus urticae, citrus red mite and vegetables, the cotton etc.
Acaricide composition with synergistic effect takes following measure to realize:
One of technical scheme of the present invention, described miticide composition are suspending agent, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Dispersant 5~20%
Antifreezing agent 0.5~3%
Thickener 0.1~2%
Defoamer 0.1~0.8%
Water surplus
The concrete production stage of this miticide composition suspending agent is earlier other auxiliary agents to be mixed, mix through high speed shear, add spiral shell mite ester and chlorfenapyr, abrading-ball is 2~3 hours in ball crusher, make a diameter all below 5mm, make the suspending agent preparation that contains the miticide composition of spiral shell mite ester and chlorfenapyr of the present invention.
Two of technical scheme of the present invention, described miticide composition are aqueous emulsion, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Emulsifier 3~30%
Solvent 5~15%
Stabilizing agent 2~15%
Antifreezing agent 1~5%
Defoamer 0.1~8%
Thickener 0.2~2%
Water surplus
The concrete production stage of this miticide composition aqueous emulsion is: at first former medicine spiral shell mite ester is added with chlorfenapyr, solvent and emulsifier, cosolvent and be in the same place, make and be dissolved into uniform oil phase; With part water, antifreeze, other insecticides adjuvant such as antimicrobial mixes into uniform water; When the reactor high speed stirs, oil phase is added water, slowly add water, open clipper and carry out high speed shear, and add remaining water, shear half an hour approximately, form the aqueous emulsion of oil-in-water type until reaching the phase inversion point.Promptly make the aqueous emulsion of the miticide composition that contains spiral shell mite ester and chlorfenapyr.
Three of technical scheme of the present invention, described miticide composition are microemulsion, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Solvent 1~30%
Emulsifier 3~30%
Stabilizing agent 2~15%
Synergist 2~10%
Water 10~78%
The concrete procedure of processing of this miticide composition microemulsion is: spiral shell mite ester and the former medicine of chlorfenapyr are added in the solvent, add auxiliary agents such as emulsifier, stabilizing agent and synergist while stirring, at last it is added in the entry and stir, form transparent and homogeneous liquid, promptly get the microemulsion of the present composition.
Four of technical scheme of the present invention, described miticide composition are wetting powder, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Dispersant 3~20%
Wetting agent 3~10%
Filler 10~70%
The concrete procedure of processing of this miticide composition wetting powder is: press above-mentioned prescription with spiral shell mite ester and chlorfenapyr and dispersant, wetting agent and filler mixing, in stirred tank, evenly stir, behind airslide disintegrating mill, mixing, promptly can be made into the wetting powder of the present composition.
Five of technical scheme of the present invention, described miticide composition are water dispersible granules, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Dispersant 3~20%
Wetting agent 3~10%
Disintegrant 2~5%
Filler 10~70%
The concrete procedure of processing of this miticide composition water dispersible granules is: by above-mentioned prescription spiral shell mite ester, chlorfenapyr and dispersant, wetting agent, disintegrant and filler are mixed, pulverize with micro jet, through mediating, add then and carry out granulation, drying, screening in the fluidized bed prilling dryer after sample analysis makes the water dispersible granules that contains the miticide composition of spiral shell mite ester and chlorfenapyr of the present invention.
Six of technical scheme of the present invention, described miticide composition are microcapsule formulations, and the percentage by weight of component is:
Spiral shell mite ester 0.1~30%
Chlorfenapyr 0.1~30%
Urea 5~20%
Formaldehyde 5~20%
Emulsifying dispersant 5~20%
Antifreezing agent 1~5%
Thickener 0.1~2%
Defoamer 0.1~0.8%
Water surplus
This miticide composition microcapsule formulations procedure of processing is: add urea and formaldehyde (amount of substance ratio be about 1: 1.5~2.0) in the there-necked flask of agitating device is housed, about pH value to 8~9 with the sodium hydroxide solution regulator solution, be warming up to 70~80 ℃ then, reaction obtains stable urea resin prepolymer.The former medicine of getting a certain amount of spiral shell mite ester and chlorfenapyr is dissolved in the cyclohexane, and adds emulsifying dispersant in solution, follows vigorous stirring, and being made into the aqueous solution that contains emulsifying dispersant is the O/W type stable emulsion of water.Above-mentioned urea resin prepolymer is added in the emulsion, regulate the pH value, polymerization reaction take place under the acid catalysis condition is wrapped oil phase substance, forms microcapsule granule.Slowly heat up, solidify, temperature is controlled at 40~50 ℃, hardening time 1h.Select to add an amount of auxiliary agent, the microcapsule suspending agent that gets final product stablely.
Described emulsifier is selected from any one or more mixtures formed with arbitrary proportion in calcium dodecyl benzene sulfonate and aliphatic acid polyethenoxy ether, alkylphenol polyoxyethylene sulfosuccinate, styryl phenol APEO, polyoxyethylene nonylphenol ether, castor oil polyoxyethylene ether, aliphatic acid polyethenoxy base ester, the polyoxyethylene aliphatic alcohol ether.
Described dispersant is selected from one or more in polycarboxylate, sodium lignin sulfonate, alkylphenol polyoxyethylene formaldehyde condensation products sulphate, alkyl benzene sulfonate calcium salt, naphthalene sulfonic acid-formaldehyde condensation product sodium salt, alkylphenol polyoxyethylene, aliphatic acid polyethenoxy ether, polyoxyethylene carboxylate, the fatty acid glyceride APEO.
Described solvent is any one or more mixed solvents formed with arbitrary proportion in dimethylbenzene or biodiesel, toluene, diesel oil, methyl alcohol, ethanol, n-butanol, isopropyl alcohol, turpentine oil, solvent naphtha, dimethyl formamide, dimethyl sulfoxide (DMSO), the water equal solvent.
Described wetting agent choosing is white: one or more in lauryl sodium sulfate, calcium dodecyl benzene sulfonate, Nekal BX, wetting and penetrating agent F, alkylnaphthalene sulfonate, alkylphenol ethoxylate, polyoxyethylene triphenylethylene phosphenylic acid salt, spaonin powder, silkworm excrement, the soapberry powder.
Described synergist is meant to have the medicament of enhancing penetration, wetting extended capability, knock down insect speed, improve the resistance of rainwater washing against power of agricultural chemicals, thereby improve a class safety, environmental protection of agricultural insecticide, miticidal effect, the New-type adjuvant of nontoxic, noresidue, optional in organic silicon pesticide synergist ZC-650 or organic silicon pesticide bleeding agent spreading agent Agrowet810c, agricultural organic silicon pesticide synergist Silwet408, azone any.
Described disintegrant is selected from: one or more in bentonite, urea, ammonium sulfate, aluminium chloride, citric acid, succinic acid, the sodium bicarbonate.
Described thickener is selected from: one or more in xanthans, CMC, hydroxyethylcellulose, methylcellulose, Magnesiumaluminumsilicate, the polyvinyl alcohol.
Described antimicrobial is selected from: one or both in Sodium Benzoate, sodium salicylate, the sodium sorbate.
Described stabilizing agent is selected from: a kind of in sodium citrate, resorcinol, the oxirane.
Described antifreeze is selected from: one or more in ethylene glycol, propane diols, glycerine, diethylene glycol (DEG), the triethylene glycol.
Described defoamer is selected from: silicone oil, silicone compound, C
10-20Saturated fat acid compounds, C
8-10In aliphatic alcohols compound and the polyoxyethylene glycerol ether one or more.
Described emulsifying dispersant comprises: wetting agent, dispersant, stabilizing agent, thickener, defoamer and antifreezing agent etc.
Described filler is selected from: one or more in kaolin, diatomite, bentonite, attapulgite, white carbon, starch, the precipitated calcium carbonate.
The invention has the beneficial effects as follows:
1, the used spiral shell mite ester of the present invention has the advantages that the ovum children holds concurrently and kills, but to becoming the mite effect bad, chlorfenapyr then is the miticide with strong stomach poison function, can prevent and treat at each vegetative stage of evil mite.
2, two kinds of composite miticides have double action mechanism, delay the drug-fast generation of evil mite.
3, reduced the agricultural chemicals usage amount, strengthened friendly environment.
Specific embodiment
The different proportioning co-toxicities of spiral shell mite ester with chlorfenapyr
1.1 reagent agent
240g/L spiral shell mite ester suspending agent, the former medicine of 95% chlorfenapyr, spiral shell mite ester and chlorfenapyr different proportion mixture, above-mentioned former medicine provides by Hunan Chemical Research Institute's pesticide research.
1.2 for examination worm source
Two-spotted spider mite.
1.3 single agent assay method
Adopt dip-slide method,, former medicine is made into 10% missible oil according to the preliminary experiment result, being diluted with water to variable concentrations, is contrast with the clear water, places the slide of the specification unanimity of getting ready the soup of variable concentrations to soak 30s respectively, dry slightly after the taking-up, put into culture dish (diameter 9cm), the two-spotted spider mite adult of criteria for selection unanimity is placed on the slide, 20 in every ware, seal with wet gauze the upper end, and each concentration repeats 3 times, totally 60.Connecing test tube behind the worm, to put into temperature be that 26 ℃, relative moisture are 70% insectary, check dead, the borer population of living behind the 48h, calculate lethality, and proofread and correct, ask virulence regression equation, the lethal dose of 50 (LC50) and correlation coefficient (r) with probability value analytical method then with the lethality of contrast.
1.4 the joint toxicity measuring method of different proportionings
According to the toxicity test result of single agent, by the active ingredient mass ratio
Spiral shell mite ester: the ratio that chlorfenapyr was respectively 3: 1,5: 1,7: 1,10: 1,20: 1 is mixed.Adopt above-mentioned 1.3 methods to carry out toxicity test, calculate LC50, and press the abundant method of Sun Yun and calculate co-toxicity coefficient (CTC).Co-toxicity coefficient CTC, computing formula is as follows: (with spiral shell mite ester is the standard medicament, and its toxicity index is 100):
LC50 * 100 of the LC50/ chlorfenapyr of the toxicity index of chlorfenapyr (TI)=spiral shell mite ester
LC50 * 100 of the LC50/M of the actual toxicity index (ATI) of M=spiral shell mite ester
TI * the P of the theoretical toxicity index (TTI) of M=spiral shell mite ester
(spiral shell mite ester)TI * the P of+chlorfenapyr
(chlorfenapyr)
TTI * 100 of the ATI/M of the co-toxicity coefficient of M (CTC)=M
In the formula:
M is a chlorfenapyr and the mixture of the different proportionings of spiral shell mite ester
P
(chlorfenapyr)Be chlorfenapyr shared ratio in mixture
P
(spiral shell mite ester)Be spiral shell mite ester shared ratio in mixture
2.1 toxicity test result
Table 1 spiral shell mite ester, chlorfenapyr are to the indoor measurement result of two-spotted spider mite
Handle title | Proportioning | Virulence regression equation (Y=a+bx) | The correlation coefficient r value | LC50(mg/L) | Co-toxicity coefficient (CTC) |
Spiral shell mite ester | - | Y=6.3129x+2.0625 | 0.9876 | 3.01 | - |
Chlorfenapyr | - | Y=5.1294+2.7406x | 0.9763 | 0.90 | - |
Spiral shell mite ester: chlorfenapyr | 3∶1 | Y=64.353-6.0977 | 0.9665 | 1.49 | 127.24 |
Spiral shell mite ester: chlorfenapyr | 5∶1 | Y=119.55x-11.896 | 0.991 | 1.3865 | 156.10 |
Spiral shell mite ester: chlorfenapyr | 7∶1 | Y=29.949x+0.6856 | 0.7484 | 1.4152 | 164.49 |
Spiral shell mite ester: chlorfenapyr | ?10∶1 | Y=10.904x+2.1137 | 0.9606 | 1.7626 | 140.77 |
Spiral shell mite ester: chlorfenapyr | ?20∶1 | Y=15.34x-0.5526 | 0.9681 | 2.3873 | 113.42 |
As can be seen from the table, in being mixed of different proportion, its co-toxicity coefficient is all greater than 120, show certain synergistic effect, wherein spiral shell mite ester: chlorfenapyr is that 7: 1 synergistic effect is the most obvious, and co-toxicity coefficient is 164.49, secondly be spiral shell mite ester: chlorfenapyr is 5: 1, and co-toxicity coefficient is 156.10.Result of the test shows that chlorfenapyr, two kinds of medicaments of spiral shell mite ester all have higher activity to two-spotted spider mite under indoor conditions, and its LC50 is respectively 0.9mg/L and 3.01mg/L.The result of the test of different proportion proportioning shows, by active ingredient spiral shell mite ester: chlorfenapyr is 3: 1,5: 1,7: 1,10: 1,20: 1 o'clock, all shows stronger synergistic effect, and wherein with spiral shell mite ester: chlorfenapyr is 5: 1~7: 1 o'clock, and synergistic effect is best.Suggestion is carried out further field control effectiveness test to the mixture preparation of 7: 1 left and right sides scopes of suitable proportion, to estimate its field practical application effect.
3 field trials are surveyed panonychus citri and two-spotted spider mite
3.1 test method
3.1.1 application method
When making up a prescription, after with low amounts of water medicament fully being dissolved earlier, add and carry out the complete stool spraying after the suitable quantity of water and handle, the sub-district spouting liquid is used by 675 liters/hectare, only sprays medicine one time.Spraying equipment is a WF-16 type knapsack hand sprayer, and shower nozzle is single fan nozzle, and operating pressure is 0.2-0.4Mpa, and spray amount is 0.36-0.48L/min, carries out the routine spraying, makes every effort to evenly thoughtful during the spray medicine.
3.1.2 investigation method
Each sub-district is at East, West, South, North, the tender tip of middle five positions mark of tree, investigate 25 movable mite quantity on the leaf altogether, hand magnifier is directly observed the blade face, investigation mite mouth radix before medicine, 1d, 7d, 14d investigate the remaining mite number alive in each sub-district respectively behind the medicine, calculate the mite mouth rate that goes down, go down rate relatively, calculate relative control effect with contrast.
3.1.3 drug effect computational methods
Mite number * 100 before the rate that goes down (%)=(mite number after the preceding several dispensers of mite of dispenser)/dispenser
Correction rate or preventive effect (%)=(the treatment region mite mouth rate of going down-check plot mite mouth go down rate)/(1-check plot mite mouth go down rate) * 100 of going down
3.1.4 poisoning investigation method
Whether continuous 14d range estimation medicament has poisoning to crop after the dispenser.
3.2 field control effectiveness test result of the test
Table 2 is handled chemical control citrus red mite (crm) field control effectiveness test result
As can be seen from Table 2, the Mixed Pharmacy of different proportion carries out field experiment by different consumptions, behind the medicine 1 day its to the control efficiency of panonychus citri and contrast medicament quite or be better than contrasting medicament, after the dispenser 7 days, its control efficiency to panonychus citri obviously was better than contrasting medicament in 15 days.According to field range estimation, in the test dose scope, plant growth is normal, and each is handled medicament and poisoning phenomenon to oranges and tangerines all do not occur, illustrates that it is safe to oranges and tangerines.In the process of the test, the test people finds that it has the better prevention effect to the oranges and tangerines blister mite.
In sum, the present invention contains the Pesticidal combination of spiral shell mite ester and chlorfenapyr, insects such as panonychus citri, oranges and tangerines blister mite there is the better prevention effect, to the target crop safety, compare with single agent, Pesticidal combination of the present invention has the advantage that quick-acting is good, the lasting period long, delay the pest resistance to insecticide generation, and the present composition does not contain organic solvents such as dimethylbenzene, be easy to transportation and use, environmental pollution is few, be difficult for producing poisoning, so research and development of the present invention and popularization have crucial meaning to society.
Claims (6)
1. miticide composition, it is characterized in that: contain chlorfenapyr and two kinds of active components of spiral shell mite ester, wherein the weight ratio of chlorfenapyr and spiral shell mite ester is 0.1~30: 0.1~30.
2. miticide composition according to claim 1 is characterized in that: the more excellent weight ratio of chlorfenapyr and spiral shell mite ester is 0.5~30: 0.5~30.
3. miticide composition according to claim 1 is characterized in that: the percentage by weight that chlorfenapyr and spiral shell mite ester are accumulated shared preparation is 1~60%.
4. miticide composition according to claim 1 is characterized in that: chlorfenapyr and spiral shell mite ester and auxiliary agent and cosolvent are re-dubbed any one formulation that allows on the agricultural chemicals.
5. miticide composition according to claim 4 is characterized in that: the formulation that can be processed into is suspending agent, aqueous emulsion, microemulsion, wetting powder, water dispersible granules and microcapsule formulations etc.
6. miticide composition according to claim 1 is characterized in that: be used to prevent and treat multiple mite class on tetranychus viennensis, apple tetranychus, panonychus ulmi, Tetranychus urticae, citrus red mite and vegetables, the cotton etc.
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Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103004769A (en) * | 2012-12-26 | 2013-04-03 | 湖南海利化工股份有限公司 | Acaricidal composition containing chlorine chlorfenapyr and spirodiclofen |
CN106035341A (en) * | 2016-06-27 | 2016-10-26 | 青岛润生农化有限公司 | Acaricidal compound containing ethyl cyanide and spirodiclofen |
Citations (3)
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CN101300979A (en) * | 2008-07-08 | 2008-11-12 | 广西田园生化股份有限公司 | Compounded pesticide composition containing Spirodiclofen |
CN101401576A (en) * | 2008-11-18 | 2009-04-08 | 深圳诺普信农化股份有限公司 | Composition for killing acarid |
CN101606517A (en) * | 2009-07-27 | 2009-12-23 | 深圳诺普信农化股份有限公司 | A kind of farm chemical emulsion preparation |
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Patent Citations (3)
Publication number | Priority date | Publication date | Assignee | Title |
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CN101300979A (en) * | 2008-07-08 | 2008-11-12 | 广西田园生化股份有限公司 | Compounded pesticide composition containing Spirodiclofen |
CN101401576A (en) * | 2008-11-18 | 2009-04-08 | 深圳诺普信农化股份有限公司 | Composition for killing acarid |
CN101606517A (en) * | 2009-07-27 | 2009-12-23 | 深圳诺普信农化股份有限公司 | A kind of farm chemical emulsion preparation |
Cited By (2)
Publication number | Priority date | Publication date | Assignee | Title |
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CN103004769A (en) * | 2012-12-26 | 2013-04-03 | 湖南海利化工股份有限公司 | Acaricidal composition containing chlorine chlorfenapyr and spirodiclofen |
CN106035341A (en) * | 2016-06-27 | 2016-10-26 | 青岛润生农化有限公司 | Acaricidal compound containing ethyl cyanide and spirodiclofen |
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Application publication date: 20110706 |