CN103651381A - Acaricidal preparation and application thereof - Google Patents

Acaricidal preparation and application thereof Download PDF

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Publication number
CN103651381A
CN103651381A CN201210358582.1A CN201210358582A CN103651381A CN 103651381 A CN103651381 A CN 103651381A CN 201210358582 A CN201210358582 A CN 201210358582A CN 103651381 A CN103651381 A CN 103651381A
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agriculture breast
mite
aqueous suspension
suspension agent
compd
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CN103651381B (en
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张国生
宋玉泉
孙克
刘少武
冯聪
高亮
于海波
李斌
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Shenyang Sinochem Agrochemicals R&D Co Ltd
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Shenyang Research Institute of Chemical Industry Co Ltd
Sinochem Corp
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Abstract

The invention belongs to the field of agricultural acaricide and relates to a water suspending agent which takes a compound A as an acaricidal active ingredient, wherein a structural formula of the compound A is shown in the specification. The water suspending agent in the invention can be used as an acaricide for preventing and treating pest mites on agriculture, forestry or hygiene, has an excellent control effect on the pest mites such as tetranychus cinabarinus boisdu adults, nymphs and mite eggs, and is safe on crops.

Description

A kind of mite-killing preparation and application thereof
Technical field
The invention belongs to miticide field, relate to a kind of vinyl cyanide miticide preparation, relate to particularly and take a kind of mite-killing preparation and the application thereof that the disclosed compound 5 of CN 101875633A is active component.
Background technology
As everyone knows, miticide has obvious effect aspect control agricultural evil mite or urban health evil mite.But miticide is in use for some time, evil mite can produce certain resistance, along with people are to growing needs and pay attention to day by days to environmental protection such as Pesticidal products, and low, the environment amenable miticide kind of active demand use cost in agricultural.The disclosed compound 5(of CN 101875633A is hereinafter to be referred as compd A) if to evil mite as Tetranychus cinnabarinus becomes the preventive effect of mite mite, the equal tool excellence of mite ovum, to crop safety, be a kind of efficient miticide, there is wide market application foreground.The structure of compd A is as follows:
Figure BDA00002181626700011
In prior art, only mention compd A and can be processed into preparation, but there is no concrete technical scheme.CN 101875633A adopts matching while using to obtain a kind of class creamy " formulation " while testing former medicine biologically active is just in order to meet the needs of biological activity test, both do not meet the requirement of Pesticide formulation specified standard, be difficult to meet the needs of practical application yet.Yet, there is no at present the report for compd A preparation research.
Summary of the invention
The object of the invention is to develop a kind of mite-killing preparation that compd A is active component of take.Due to aqueous suspension agent, not only there is the advantages such as particle diameter is little, good dispersion, good fluidity, suspensibility is high, biologically active is high, using dosage is little, and have resistance of rainwater washing against, residual low, to advantages such as people and animals' low toxicities, the simultaneously production of aqueous suspension agent with use in without dust drift, nonflammable explosive, safety good, be easy to packing, transportation and storage, therefore object of the present invention be take the miticide aqueous suspension agent that compd A is active component for exploitation is a kind of, to meet agricultural production practical application, to bring into play former medicine biologically active, effectively control evil mite better.
In order to realize object of the present invention, inventor is according to its action target and application mode, and the suitable auxiliary agent mating with active ingredient by screening, has determined a kind of miticide aqueous suspension agent formula.This aqueous suspension agent can improve wetting, spread, dispersion, delay and the permeance property of active ingredient on crop target, reaches the object that improves its acaricidal activity, reduces use cost, preserves the ecological environment, thereby has realized object of the present invention.
Agricultural chemicals itself is that a class has bioactive speciality chemical, and the auxiliary agent of dissimilar, different chemical structures, has considerable influence to the activity of compd A.Same target crop, is used different surfactants, and its assimilation effect is also not quite similar, and the difference in this activity of being brought by this body structure of surfactant is difficult to compensation by the way that improves concentration.Outstanding feature of the present invention is exactly by the adjuvant system of selecting and interpolation is mated with compd A, this adjuvant system contributes to active ingredient solubilising and dispersed pesticide activity component particle external surface and porous surface is had to good wetting action, be adsorbed in the surface of former medicine particle, form the adsorption layer of comparatively dense, interaction with " steric hindrance " makes mutually to repel between particle, thereby make it dispersed, can also stop agricultural chemicals particle to be assembled once again in adjustment and storage period, make it keep a kind of good dispersiveness, appearance stability and heat storage stability, reduce rate of crystalline growth.The dilution of said preparation has higher plate-out ability and adhesivity on control target simultaneously; thereby obviously improve wetting, spread, dispersion, delay and the permeance property of its liquid; reduce spray liquor (air-flow) drift with the wind; thereby being beneficial to liquid sprawls on blade face and sticks; reach and improve its biologically active; the effective ingredient consumption that significantly reduces agricultural chemicals, reduces costs, the object of preserving the ecological environment.
The selected auxiliary agent kind of aqueous suspension agent of the present invention is good to Environmental compatibility, does not increase former medicine to mammiferous toxicity, and crop is not produced to poisoning; Pesticide original medicine is possessed to good chemical stability; Do not reduce the biologically active of pesticide active ingredient; In use can improve the dispersity of active ingredient and active ingredient to the deposition of target body and deposition ratio; Consumption is few, to the strong adaptability of operation technique condition.
Technical scheme of the present invention is as follows:
A miticide aqueous suspension agent, take compd A as active component, contains dispersant, antifreezing agent and water in preparation; In described aqueous suspension agent, the weight percentage of each component is: compd A 0.5~70%, dispersant 1~50%, antifreezing agent 1~20%, water 5~90%.
The comparatively preferred technical scheme of the present invention is:
In miticide aqueous suspension agent, the weight percentage of each component is: compd A 5~50%, dispersant 5~30%, antifreezing agent 1~10%, water 15~80%.
Further preferred technical scheme is:
In miticide aqueous suspension agent, the weight percentage of each component is: compd A 10~30%, dispersant 8~20%, antifreezing agent 2~8%, water 45~80%.
The dispersant kind relating in miticide aqueous suspension agent formula of the present invention all has report in the monograph of the relevant surfactant of multi-section and formulations of pesticide processing.For example, < < surfactant science and application > >, the chief editors such as Jiang Qingzhe, Sinopec publishing house, 2009; < < special surfactant > >, the chief editors such as Wang Peiyi, China Textiles Press; < < formulations of pesticide process technology > >, Liu Bulin chief editor, Chemical Industry Press, 1998; Sisely nd Wood, Encyclopedia of Surface Active Agents, Chemical Publ., Co., Inc., New York, 1964.
Particularly, the dispersant in miticide aqueous suspension agent of the present invention can be selected from: the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, agriculture breast 0201B, agriculture breast 0203B, agriculture breast 100 #, agriculture breast 500 #, Nongru-700 #, agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast OX-635, agriculture breast OX-662, sodium lignin sulfonate, Nekal BX, detergent LS, calcium lignosulfonate, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate, methanonaphthalene sodium sulfonate, oleic acid methylamino ethylsulfonic acid sodium, alkyl-diethylene glycol ether-sodium sulfonate, N-methyl-oleoyl-sodium taurocholate, dibutyl naphthalene sulfonic acid-formaldehyde condensation product, epoxidized polyether, to tertbutyl ether, castor oil ethylene oxide adduct, ethylene oxide-propylene oxide block copolymer, alkylphenol polyoxyethylene formaldehyde condensation products, one or more in alkylphenol-polyethenoxy polyethenoxy ether or methylcellulose.Also the available PICO series of products of Japanese Zhu Ben's Oil Corporation of selecting are if PICO-LF1, PICO-LF3, PICO-LF7, PICO-LF1, PICO-LPQ are as dispersant.
Further preferred dispersant is: the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast 0201B, agriculture breast 0203B, Nongru-700 #, one or more in agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate or methanonaphthalene sodium sulfonate.
Antifreezing agent in miticide aqueous suspension agent of the present invention can be selected from: ethylene glycol, glycerine, propane diols, polyethylene glycol, sorbierite or urea.
Further preferred antifreezing agent is ethylene glycol or glycerine.
In addition, in some situation, add appropriate thickener can improve the physical stability of aqueous suspension agent, as reduced layering, being convenient to packing.Thickener in miticide aqueous suspension agent of the present invention can be selected from: one or more in xanthans, gelatin, gum Arabic, polyvinyl acetate, polyvinylpyrrolidone, aluminium-magnesium silicate, polyvinyl alcohol, polyethylene glycol, phenolic resins, shellac, CMC, hydroxyethylcellulose, hydroxypropyl cellulose, methylcellulose and sodium alginate.Yet part dispersant also can have the effect of thickener in some situation.
In miticide aqueous suspension agent of the present invention, when polysaccharose substance (in formula, contain the material that easily goes mouldy for example) adds a small amount of preservative can improve the situation of easily going mouldy when aqueous suspension agent is stored in some cases, and preservative can be selected from conventionally: one or more in Sodium Benzoate, Kathon CG (MIT with (B) CMIT), potassium sorbate, dehydro sodium acetate, calcium propionate, sodium Diacetate, sodium lactate, propylparaben.
While preparing aqueous suspension agent, sometimes owing to easily air being brought in plant equipment reason and process, produce bubble, conventionally need to add appropriate defoamer.Defoamer in miticide aqueous suspension agent of the present invention can be selected from: bubble enemy, silicone oil, silicone, WJX-1, C 8~10fatty alcohol, C 10~20saturated fat acids (as capric acid, stearic acid etc.) or C 10~20unsaturated fatty acid amide.The selection of defoamer is appreciated by those skilled in the art.
The miticide aqueous suspension agent the present invention relates to adopts conventional method preparation, its compound method is: compd A is joined in blending tank and mixed with dispersant, antifreezing agent and water ratio on demand, first pass through high-speed shearing machine coarse crushing, then be pumped into and in sand mill, carry out fine grinding, when the average grain diameter of 95% material reaches 5 μ m particle diameters when following, filter, can obtain miticide aqueous suspension agent product of the present invention.
Adopt the aqueous suspension agent that contains active constituent compound A of formulated of the present invention, biologically active is excellent, and its acaricidal activity is significantly better than the measurement result of former medicine is provided by the method providing in CN 101875633 A.
Miticide aqueous suspension agent of the present invention can, before use through diluting or being directly watered spraying, also can directly be used.
Technical scheme of the present invention also comprises the method for control evil mite: miticide aqueous suspension agent of the present invention is imposed on described harmful mite or its somatomedin.Conventionally the comparatively suitable effective dose of selecting is 10 grams to 1000 grams of per hectares.
Technical scheme of the present invention also comprises the purposes of above-mentioned miticide aqueous suspension agent: for the preparation of the purposes of killing mite aqueous suspension agent medicine, miticide aqueous suspension agent of the present invention can be applicable to the control of Agricultural Mites, forestry harmful mites or non-therapeutic purposes health evil mite, if especially evil mite is become to the preventive effect of mite mite, the equal tool excellence of mite ovum as Tetranychus cinnabarinus, to crop safety.
Miticide aqueous suspension agent of the present invention has the following advantages: 1) flash-point is high, nonflammable, explosive, stores, uses safety; 2) dust is few, and environmental pollution is little, uses conveniently, to the producer and user and Environmental security; 3) aqueous suspension agent be take water as matrix, aboundresources, and product cost is low, easily packing; 4) have a particle diameter little, good dispersion, good fluidity, suspensibility is high, biologically active is high, using dosage is little, resistance of rainwater washing against, residual low, to features such as people and animals' low toxicities; 5) after aqueous suspension agent spraying, with fine particle, be distributed in crop surface, miticidal effect is good; 6) saving of labor, save time, with rational application mode, minimum drug cost, can reach the object of pest control.
Embodiment
Following specific embodiment is used for further describing the present invention, but the present invention is limited to absolutely not these examples.In formula, percentage and umber are all by weight.Active constituent compound A self-control (content 98%), folding hundred post doses add, and other each raw materials are commercially available product.
Pharmaceutical formulation embodiment
Embodiment 1,10% compd A aqueous suspension agent
Figure BDA00002181626700041
Compound method is as follows: above-mentioned substance is joined in blending tank and mixed successively, first through high shear, carry out coarse crushing, homogenize, then be pumped into and in sand mill, carry out fine grinding, particles distribution instrument detects the granularity of sand milling material, when particle diameter reaches after (by 75 μ m standard screen >=98%) standard-required, filter, can obtain 10% compd A aqueous suspension agent.Following formulation Example is preparation in the same way all.
Embodiment 1 sample all technical is: pH value 6.3; Suspensibility 93.8%; Pourability: topple over rear residue 3.5%, residue 0.2% after washing; Lasting foaming characteristic (after 1min) 30mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.0%.
Embodiment 2,10% compd A aqueous suspension agent
Figure BDA00002181626700042
Embodiment 2 sample all technicals are: pH value 6.5; Suspensibility 96.5%; Pourability: topple over rear residue 3.8%, residue 0.2% after washing; Lasting foaming characteristic (after 1min) 25mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.1%.
Embodiment 3,20% compd A aqueous suspension agent
Figure BDA00002181626700051
Embodiment 3 sample all technicals are: pH value 6.6; Suspensibility 95.9%; Pourability: topple over rear residue 3.9%, residue 0.3% after washing; Lasting foaming characteristic (after 1min) 30mL; Low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.3%.
Embodiment 4,20% compd A aqueous suspension agent
Embodiment 4 sample all technicals are: pH value 6.2, and suspensibility 94.8%, pourability: topple over rear residue 3.6%, residue 0.3% after washing, lasting foaming characteristic (after 1min) 28mL, low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.5%.
Embodiment 5,30% compd A aqueous suspension agent
Figure BDA00002181626700053
Embodiment 5 sample all technicals are: pH value 6.6, and suspensibility 93.6%, pourability: topple over rear residue 3.8%, residue 0.3% after washing, lasting foaming characteristic (after 1min) 31mL, low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 0.8%.
Embodiment 6,30% compd A aqueous suspension agent
Figure BDA00002181626700062
Embodiment 6 sample all technicals are: pH value 6.3, and suspensibility 95.1%, pourability: topple over rear residue 4.0%, residue 0.3% after washing, lasting foaming characteristic (after 1min) 27mL, low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.2%.
Embodiment 7,30% compd A aqueous suspension agent
Figure BDA00002181626700063
Figure BDA00002181626700071
Embodiment 7 sample all technicals are: pH value 6.8, and suspensibility 92.9%, pourability: topple over rear residue 3.5%, residue 0.2% after washing, lasting foaming characteristic (after 1min) 20mL, low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.0%.
Embodiment 8,30% compd A aqueous suspension agent
Figure BDA00002181626700072
Embodiment 8 sample all technicals are: pH value 6.5, and suspensibility 95.2%, pourability: topple over rear residue 3.2%, residue 0.2% after washing, lasting foaming characteristic (after 1min) 22mL, low-temperature stability is qualified; Heat storage stability (54 ± 2) ℃/14 days, resolution ratio is 1.1%.
Performance test embodiment
Embodiment 9, stability comparative trial
Mite-killing preparation of the present invention is mixed with to the aqueous suspension agent of desired concn according to conventional method, tests its stability.
With the method preparation compd A that provides in CN 101875633A in contrast preparation carry out comparative trial.The preparation of control formulation: acetone solution for compd A (content of acetone in total solution is no more than 10%), is then mixed with the solution of desired concn with 0.1% the Tween 80 aqueous solution.
Test result is in Table 1.
Table 1. stability comparative test result (normal temperature)
Figure BDA00002181626700073
Figure BDA00002181626700081
As seen from the above table, control formulation normal temperature is placed after 1 month and can not be used again; And preparation provided by the invention (embodiment 2, embodiment 4 of take is example with the aqueous suspension agent of embodiment 5 preparations) was placed after 1,6,12 month, surface tension all changes not quite, by 98% average grain diameter (d 98) change also little.This shows that aqueous suspension agent of the present invention not only all can meet liquid soaking on target, and As time goes on, levigate particle does not change substantially yet.Finer particles, drug effect are better, otherwise, drug effect performance is poorer.Upper table data acknowledgement select the aqueous suspension agent of adjuvant system of the present invention preparation, use conveniently, be beneficial to the performance of drug effect.
Biological activity test embodiment
Embodiment 10, biologically active comparative trial
The compound method of suspending agent and former medicine is the same.
Test method: the test sample that adopts potted plant seedling spray-on process to measure different batches becomes the activity size of mite to Tetranychus cinnabarinus.First Tetranychus cinnabarinus of the same size is become mite to receive on the Tolerance of Kidney Bean Seedlings blade in first pair of open and flat phase of true leaf, after becoming mite stable, count radix; Then press the order even spraying of experimental scheme from low dosage to high dose, every strain 2mL, every processing repeats for 3 times, separately establishes blank.The observation ward that examination material after processing is placed in to certain condition, periodic investigation becomes mite number anyway, calculates lethality.
Table 2 part embodiment formulation samples acaricidal activity measurement result
Figure BDA00002181626700082
--*: represent not survey

Claims (10)

1. a mite-killing preparation, is characterized in that: the aqueous suspension agent that the compd A of take is active component, and in preparation, key component and weight percentage are:
Compd A 0.5~70%,
Dispersant 1~50%,
Antifreezing agent 1~20%,
Water 5~90%;
Compd A structural formula is as follows:
Figure FDA00002181626600011
2. mite-killing preparation according to claim 1, is characterized in that: in described aqueous suspension agent, the weight percentage of key component is: compd A 5~50%, dispersant 5~30%, antifreezing agent 1~10%, water 15~80%.
3. mite-killing preparation according to claim 2, is characterized in that: in described aqueous suspension agent, the weight percentage of key component is: compd A 10~30%, dispersant 8~20%, antifreezing agent 2~8%, water 45~80%.
4. according to the mite-killing preparation described in claim 1-3 any one, it is characterized in that: the dispersant of preparation aqueous suspension agent is selected from the sodium salt of alkyl naphthalene sulfonic acid condensation polymer, agriculture breast 0201B, agriculture breast 0203B, agriculture breast 100 #, agriculture breast 500 #, Nongru-700 #, agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast OX-635, agriculture breast OX-662, sodium lignin sulfonate, Nekal BX, detergent LS, calcium lignosulfonate, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate, methanonaphthalene sodium sulfonate, oleic acid methylamino ethylsulfonic acid sodium, alkyl-diethylene glycol ether-sodium sulfonate, N-methyl-oleoyl-sodium taurocholate, dibutyl naphthalene sulfonic acid-formaldehyde condensation product, epoxidized polyether, to tertbutyl ether, castor oil ethylene oxide adduct, ethylene oxide-propylene oxide block copolymer, alkylphenol polyoxyethylene formaldehyde condensation products, one or more in alkylphenol-polyethenoxy polyethenoxy ether or methylcellulose.
5. mite-killing preparation according to claim 4, is characterized in that: described dispersant is selected from sodium salt, agriculture breast NP-7, agriculture breast NP-8, agriculture breast NP-15, agriculture breast 0201B, agriculture breast 0203B, the Nongru-700 of alkyl naphthalene sulfonic acid condensation polymer #, one or more in agriculture breast BY110, agriculture breast 1601, agriculture breast T-20, agriculture breast S-80, methyl naphthalene sulfonate formaldehyde condensate, naphthalenesulfonic acid-formaldehyde condensate or methanonaphthalene sodium sulfonate.
6. according to the mite-killing preparation described in claim 1-3 any one, it is characterized in that: described antifreezing agent is selected from ethylene glycol, glycerine, propane diols, polyethylene glycol, sorbierite or urea.
7. mite-killing preparation according to claim 6, is characterized in that: described antifreezing agent is selected from ethylene glycol or glycerine.
8. according to the mite-killing preparation described in claim 1-3 any one, it is characterized in that: in described aqueous suspension agent, can also add appropriate thickener, preservative and/or defoamer as required.
9. a method of controlling harmful mite, is characterized in that, the mite-killing preparation described in claim 1-3 any one is imposed on and needed on the harmful mite of control or the medium of its growth with 10~1000 grams of active ingredient/hectares.
10. the mite-killing preparation as described in claim 1-3 any one is in the purposes of preventing and treating evil mite in agricultural, forestry or health.
CN201210358582.1A 2012-09-24 2012-09-24 A kind of mite-killing preparation and application thereof Active CN103651381B (en)

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CN106305727A (en) * 2015-06-18 2017-01-11 沈阳中化农药化工研发有限公司 Synergist-containing insecticidal acaricidal composition
CN108684681A (en) * 2017-03-31 2018-10-23 沈阳中化农药化工研发有限公司 A kind of mite-killing preparation and its application
CN108949373A (en) * 2018-06-29 2018-12-07 东莞市硕丰研磨科技有限公司 Glass cleaner
CN109479883A (en) * 2014-12-25 2019-03-19 沈阳中化农药化工研发有限公司 Insecticidal and acaricidal composition of the one kind containing fungicide or bactericidal (virus) agent
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CN114762502A (en) * 2021-01-13 2022-07-19 沈阳中化农药化工研发有限公司 Acaricide suspending agent and preparation thereof

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Cited By (10)

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Publication number Priority date Publication date Assignee Title
CN109479883A (en) * 2014-12-25 2019-03-19 沈阳中化农药化工研发有限公司 Insecticidal and acaricidal composition of the one kind containing fungicide or bactericidal (virus) agent
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CN106305727B (en) * 2015-06-18 2019-02-15 沈阳中化农药化工研发有限公司 A kind of insecticide acaricide composition containing synergist
CN105875659A (en) * 2016-05-17 2016-08-24 梁文荣 Pesticide preparation for killing spider mite
CN108684681A (en) * 2017-03-31 2018-10-23 沈阳中化农药化工研发有限公司 A kind of mite-killing preparation and its application
CN108684681B (en) * 2017-03-31 2021-03-30 沈阳中化农药化工研发有限公司 Mite killing preparation and application thereof
CN108949373A (en) * 2018-06-29 2018-12-07 东莞市硕丰研磨科技有限公司 Glass cleaner
CN111789122A (en) * 2019-04-09 2020-10-20 浙江省化工研究院有限公司 Acaricidal composition containing oxapyrile-acarbonitrile and spirocyclic tetronic acid pesticide
CN114762502A (en) * 2021-01-13 2022-07-19 沈阳中化农药化工研发有限公司 Acaricide suspending agent and preparation thereof
CN114762502B (en) * 2021-01-13 2023-03-21 沈阳中化农药化工研发有限公司 Acaricide suspending agent and preparation thereof

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