CN110250190A - A kind of composition, preparation and its application, preparation method - Google Patents

A kind of composition, preparation and its application, preparation method Download PDF

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Publication number
CN110250190A
CN110250190A CN201910662007.2A CN201910662007A CN110250190A CN 110250190 A CN110250190 A CN 110250190A CN 201910662007 A CN201910662007 A CN 201910662007A CN 110250190 A CN110250190 A CN 110250190A
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China
Prior art keywords
agent
preparation
composition
stabilizer
active constituent
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CN201910662007.2A
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Chinese (zh)
Inventor
李义涛
姚强
梁任龙
刘新烁
陈锦昌
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Dongguan Dongyangjunyang Hydrogen Patent Pesticide Co ltd
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Dongguan Dongyang Guangke Research and Development Co Ltd
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Priority to CN201910662007.2A priority Critical patent/CN110250190A/en
Publication of CN110250190A publication Critical patent/CN110250190A/en
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings
    • A01N43/42Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom six-membered rings condensed with carbocyclic rings
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION 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
    • A01N43/00Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/647Triazoles; Hydrogenated triazoles
    • A01N43/6531,2,4-Triazoles; Hydrogenated 1,2,4-triazoles

Abstract

The present invention relates to a kind of composition, preparation and its applications, preparation method.A kind of composition, including drug activity component;The drug activity component includes active constituent a and active constituent b, the active constituent a are olefin conversion, and the active constituent b is Ipflufenoquin.The composition is applied widely, effect is good, at low cost, residual is low as fungicide, and safe for human, animal and environment, two kinds of active components show brilliant synergistic function in preventing and treating fungus-caused cereal crop related disease.

Description

A kind of composition, preparation and its application, preparation method
Technical field
The present invention relates to pesticide field, in particular to a kind of composition, preparation and its application, preparation method.
Background technique
Ipflufenoquin is a kind of quinolines fungicide developed by Japanese Nippon-Soda company.Develop code name NF-180, Chinese chemical name are known as 2- [(7,8- bis- fluoro-2-methyl-3-quinolin base) oxygroup] -6- fluoro- a, a- dimethyl benzene first Alcohol, entitled [2- [(7,8-difluoro-2-methyl-3-quinolinyl) the oxy] -6-fluoro-a, a- of English language Chemical Dimethylbenzenemethanol], CAS accession number is 1314008-27-9, and structural formula is as follows:
Olefin conversion is triazole bactericidal agent, inhibits 14 alpha-methylated effects in the ergosterol biosynthesis of fungi, draws It plays ergosterol to lack, causes fungal cell membrane abnormal, final fungi is dead, and the lasting period is permanent.Olefin conversion is to people and animals, beneficial Insect, Environmental security, and Chinese chemical name referred to as (E)-(RS) -1- (2,4- dichlorophenyl) -4,4- dimethyl -2- (1H-1,2,4- Triazol-1-yl) amyl- 1 alkene -3- alcohol, olefin conversion structural formula is as follows:
Chemical agent is the effective means for preventing and treating wheat powdery mildew.Since resistance of the current wheat powdery mildew to pesticide is more next It is stronger, cause the usage amount of pesticide to increase year by year, so that the pollution to environment is increasingly severe.
Therefore, it is badly in need of developing the significant composition pesticide of a kind of pair of wheat powdery mildew control efficiency at present.
Summary of the invention
The first object of the present invention is to provide a kind of composition, the composition mainly by olefin conversion with Ipflufenoquin composition not only solves the problem that prior art dosage is excessively high, preventive effect is insufficient, and has sterilization It composes wider, quick-acting and long-acting and other effects.
The second object of the present invention is to provide a kind of preparation, and preparation type is extensive, equally can solve prior art medication Excessively high and insufficient preventive effect problem is measured, can achieve the effect that expand fungicidal spectrum, quick-acting and long-acting.
In order to achieve the goal above, the present invention provides following technical schemes:
A kind of composition, including drug activity component;The drug activity component includes active constituent a and active constituent b, The active constituent a is olefin conversion, and the active constituent b is Ipflufenoquin.
In some embodiments, in the present composition, the drug activity component is by active constituent a and active constituent B composition, the active constituent a are olefin conversion, and the active constituent b is Ipflufenoquin.
It is a discovery of the invention that after combining olefin conversion with Ipflufenoquin ideal disease pest can be reached with lower dose Evil control efficiency, and show good quick-acting and long-term effect.
Specifically, the present invention at least can reach addition bactericidal effect (to the co-toxicity coefficient of wheat powdery mildew 82 with On), and fungicidal spectrum is widened to other cereal crop pathogens (such as resistant strain of cereal crop disease);Reduce activation Close the rate of application of object;Even if shown in single compound it is inactive or almost without under active rate of application, by work of the invention Property combinations of compounds is still enough to prevent and treat pathogen;In preparation or use process (such as grind, screening, emulsification, dissolve or divide Dissipate) advantageous feature;The storage stability and photostability of enhancing;Advantageous residue is formed;Improved toxicology and ecology Toxicological profile;Can provide improved cereal crop characteristic, for example, preferably grow, improve the tolerance to high temperature or low temperature, Improve the tolerance to arid or water or soil salt content, improve Flowering quality, make to bloom earlier, hasting of maturity, raising adopt Receive yield, more flourishing root system, bigger fruit, higher cereal plant height, bigger leaf area, greener leaf, more Strong spray, less seed demand, lower cereal crop toxicity, the transfer of cereal crop system of defense and cereal makees The good compatibility of object, the quality of harvested products is higher and/or nutritive value is higher, the sugared concentration in fruit is higher, harvesting produces The storage stability and/or processability of product are more preferable;Importantly, synergy can be played after proportion combination appropriate Effect;Can delay the generation of drug resistance simultaneously, improve the safety to crop, two kinds of agriculture chemical compoundings also reduce medication at This, saves labour.
If olefin conversion and Ipflufenoquin can be respectively with alloisomerism, optical siomerism or tautomerisms in the present invention Form exist, then it should be understood that even if being not expressly mentioned in each example, under usable condition, such compound is within a context It further include corresponding isomeric form.
The mass ratio of active constituent a and active constituent b are arbitrary in the present invention.
For example, the mass ratio of active constituent a and active constituent b can change in relatively wide range, it is certain preferred Embodiment in mass ratio be 1~30: 30~1, more preferable 1~15: 15~1, more preferable 1: 1~15,1~5: 5~1 or 1: 1~5, it can reach the effect of more significant synergy in the preferred scheme, co-toxicity coefficient reaches 120 or more, optional matter Amount ratio has 15:1,13:1,12:1,10:1,8:1,7:1,6:1,5:1,4:1,3:2,1:1,1:2,1:3,1:4,1:5,1:6,1: 7,1:8,1:9,2:3,2:5,2:7,3:4,3:5,3:7,1:10,1:11,1:12,1:13,1:14 or 1:15.Wherein preferred model Be with: (1:30)~(15:1), (1:30)~(10:1), (1:30)~(5:1), (1:30)~(3:1), (1:30)~(2:1), (1:30)~(1:1), (1:15)~(30:1), (1:15)~(15:1), (1:15)~(10:1), (1:15)~(5:1), (1: 15)~(3:1), (1:15)~(2:1), (1:15)~(1:1), (1:10)~(20:1), (1:10)~(15:1), (1:10)~ (10:1), (1:10)~(5:1), (1:10)~(3:1), (1:10)~(2:1), (1:10)~(1:1), (1:5)~(20:1), (1:5)~(15:1), (1:5)~(10:1), (1:5)~(5:1), (1:5)~(3:1), (1:5)~(2:1), (1:5)~(1: 1), (1:3)~(20:1), (1:3)~(15:1), (1:3)~(10:1), (1:3)~(5:1), (1:3)~(3:1), (1:3) ~(2:1), (1:3)~(1:1), (1:2)~(20:1), (1:2)~(15:1), (1:2)~(10:1), (1:2)~(5:1), (1:2)~(3:1), (1:2)~(2:1), (1:2)~(1:1), (1~20): 1, (1~15): 1, (1~10): 1, (1~5): 1, (1~3): 1 or (1~2): 1.When content >=olefin conversion content of Ipflufenoquin, it can reach significant collaboration and increase The effect of effect, co-toxicity coefficient reach 120 or more.
Composition of the invention exceptionally, can also contain common adjuvant on pesticide, adjuvant is agriculture except drug activity group It is added in medicine preparation processing or use, for improving the auxiliary substance of medicament physicochemical property, the basic inanimate object of auxiliary agent itself is living Property, but control efficiency can be influenced.The adjuvant may include wetting agent, dispersing agent, emulsifier, thickener, disintegrating agent, prevent Freeze at least one of agent, defoaming agent, solvent, preservative, stabilizer, synergist, carrier etc., preferably includes wetting agent, dispersion In agent, emulsifier, thickener, disintegrating agent, antifreezing agent, defoaming agent, solvent, preservative, stabilizer, synergist and carrier at least It is a kind of.It can be properly added the above adjuvant according to the needs of preparation, can be varied according to different situations, special limit is had no It is fixed.
Preferably, the wetting agent is selected from alkyl phenol polyoxyethylene ether (such as nonylphenol polyoxyethylene ether, octyl phenol polyoxy Vinethene, dodecane phenolic ether, dinonyl phenolic ether and mixing alkane phenolic ether etc.), fatty acid or aliphatic ester sulfate, alkyl naphthalene sulfonic acid Salt (such as nekal, isopropyl naphthalene sulfonate), alkylbenzene sulfonate (such as neopelex, 12 Alkyl benzene calcium sulfonate), one in alkyl sulfate and lignosulfonates (such as sodium lignin sulfonate, calcium lignosulfonate) etc. Kind is a variety of.Suitable wetting agent isOTB (dioctyl sulfosuccinate),EFW (alkylation Naphthalene sulfonate),BX (alkylated naphthalene sulfonate) orMT 804 (alkylated naphthalene sulfonate).
The dispersing agent be selected from naphthalene sulfonate, naphthalenesulfonate formaldehyde condensation compound, lignosulfonates, alkylbenzene sulfonate, APES formaldehyde condensation products sulfat, polymeric polycarboxylic acid salt, alkylbenzene polyoxyethylene ether, ethylene oxide epoxy One of propane block polyether and organophosphorus ester etc. are a variety of.For wettable powders preparation, common dispersing agent For sodium lignin sulfonate (sodium lignosulphonate).For suspension concentrate, polyelectrolyte is used (polyelectrolyte) such as naphthalenesulfonic acid-formaldehyde condensate (sodium naphthalene sulphonate Formaldehyde condensate) obtain absorption and stabilization.Also tristyrylphenol ethoxylates phosphorus is used Acid esters (tristyrylphenol ethoxylate phosphate ester).The Typical Representative of suitable dispersing agent is especially2700、2500、2510、YUS-EP60P、SP-3498D、4894, Ufoxane NA, Morwet D425, GY-D800, Antraox B/848, Morwet D-425 or Ethylan NS-500LQ。
The emulsifier is selected from castor oil polyoxyethylene ether, fatty alcohol polyoxyethylene ether, alkyl phenol polyoxyethylene ether, alkyl Phenol polyethenoxy polyethenoxy ether, fatty amine, the ethylene oxide adduct of fatty acid amide, polyoxyethylene carboxylate, castor oil Ethylene oxide adduct and its derivative, rosin acid ethylene oxide adduct and the like, polyol fatty acid and its epoxy second One of alkane addition product and polyoxyethylene polyoxypropylene block copolymer etc. are a variety of.The Typical Representative of suitable dispersing agent is outstanding It is the high-purity modified lignosulphonate of lignin A, 3A, agriculture breast 500#, agriculture breast 601#, agriculture breast 602#, Nongru-700 #, agriculture breast 1601#, agriculture breast 1602#, TERMUL 2507, EMULPON CO-360 or Ethylan 992.
It is fine that the thickener is selected from white carbon black, kaolin, bentonite, xanthan gum, Arabic gum, polyacrylic acid and carboxymethyl Tie up one of plain sodium etc. or a variety of.
The disintegrating agent is in urea, modified starch, bentonite, aluminium chloride, ammonium sulfate, succinic acid, sodium bicarbonate etc. It is one or more.
The antifreezing agent is selected from one of glycerine, ethylene glycol, propylene glycol etc. or a variety of.
The defoaming agent is selected from organosilicon ketone defoaming agent, organic silicon defoaming agent (such as ETXP-40), C8-10Fatty alcohol One of class defoaming agent, polyureas and cithrol etc. are a variety of.
The solvent is toluene, dimethylbenzene, cyclohexanone, aromatic solvent, methanol, ethyl acetate, soybean oil, epoxy soybean One of oil, castor oil, corn oil, epoxy corn oil, methyl oleate, rapeseed oil and n-octylpyrrolidone etc. are a variety of.
The preservative is selected from one of sodium benzoate, benzoic acid, potassium sorbate, Kathon CG etc. or a variety of.
The stabilizer is selected from phosphoric acid, pyrophosphoric acid, neck phthalic acid, benzoic acid, triphenyl phosphite, aceticanhydride, epoxy chlorine One of propane, aluminium-magnesium silicate, resorcinol and sodium citrate etc. are a variety of.
Synergist inactive itself, but the intracorporal detoxication enzyme of biology, when with certain combined use of pesticides, energy can be inhibited Increase substantially one of pesticide virulence and drug effect, such as Synergistic Phosphorus, Butacide or a variety of.
The carrier be selected from kaolin, clay, talcum, chalk, quartz, Attagel, montmorillonite, diatomite, silica, Aluminium oxide, natural or synthetic silicates, resin, wax, solid fertilizer, water, alcohol (especially butanol), organic solvent, mineral oil and plant One of object oil and its derivative etc. are a variety of.
Additionally, if appropriate, other additional components also may be present, for example, it is protective colloid, adhesive (binder), viscous Agent (adhesive), thixotroping substance, bleeding agent, chelating agent, complexing forming agent, coloring agent etc..In general, the active ingredient Object can be in conjunction with any solid or liquid additive that are usually used in preparation purpose.
In composition of the invention, the total content (referring both to mass percent) of drug activity component in the composition is preferably 0.05-99%, 0.01-98% or 1~95%, for example, 1.0wt.%, 5.0wt.%, 10.0wt.%, 15.0wt.%, 20.0wt.%, 30.0wt.%, 40.0wt.%, 50.0wt.%, 60.0wt.%, 70.0wt.%, 80.0wt.%, 90.0wt.%, if may be 100wt.% without auxiliary agent.Wherein preferred range has 20~80wt.%, more preferable 30~ 60wt.%.
Composition of the invention not only include ready-to-use composition (can be used suitable device be applied to plant or Seed), and include commercially available concentrate (must be diluted with water before use).
The present invention also provides preparation made of above-mentioned composition, said preparation can be aerosol, capsule suspension, harl Change concentrate, heat atomization concentrate, with the particle of encapsulated, fine grained, the flowable concentrate for handling seed, at any time Available solution, can dusts powders, emulsifiable concentrate, oil in water emulsion, water-in-oil emulsion, bulky grain, microparticle, oil dispersed Property powder, oil-soluble flowable concentrate, oil soluble liquid, foam, paste, the coated seed of insecticide, suspending concentrate, outstanding Emulsion concentrate, solubility concentrate, suspension, wettable powder, soluble powder, powders and granules, water-soluble granular Or tablet, the water solube powder for handling seed, wettable powder, natural products and the synthetic impregnated with reactive compound Microencapsulation and ULV harl and hot atomization preparation in the coating material of matter and polymeric material and seed.Preferred system Agent includes missible oil, wettable powder, suspending agent, granule, water dispersion granule, microemulsion, aqueous emulsion or microcapsule formulations.
Pulvis (DP) is that a certain amount of inert dust, such as clay, kaolin, talcum powder is added in active material, is added through machinery Work is at powdered object, and powder diameter is at 100 μm or less.
Wettable powder (WP) refer to by composition by a certain percentage with suitable surfactant and inert substance (kaolinite Native powder) mixture.Wettable powder is the preparation for caning be uniformly dispersed Yu Shuizhong, wherein in addition to active constituent and inert substance Other than (kaolin powder), also containing a certain amount of anion or nonionic surface active agent (dispersing agent, wet benefit).
Microcapsule formulations (MC) are first to be coated on active matter to form small cryptomere preparation in adhesive, film forming agent etc., so It is reprocessed into the dosage form of needs afterwards;It is divided into micro-capsule suspension (Capsule Suspensions, CS) and microcapsules granula (Encapsulated Granule, CG), microcapsules dry suspending agent (Capsulated Dry Flowable, CDF) etc..
Water dispersion () granula (WDG) refer to by composition by a certain percentage with suitable surfactant and inert substance The mixture of (kaolin) powder.Through air-flow crushing, particle size is made to reach requirement, and uses double helical form mixing machine and colter Formula mixing machine keeps product mix uniform through repeatedly mixing, then by conventional method as fluidized bed prilling, mist projection granulating, disc type are made Grain.
Granule (GR) refer to by composition by a certain percentage with suitable surfactant, diluent and inert substance The mixture of (kaolin powder).It is granulated such as fluidized bed prilling method by pelletizer, is to keep powder under flow regime, spray Mist binder solution is allowed to the prilling process being aggregated.This method makes the processes such as mixing, kneading, granulation, dry, classification one In a device, the short time is completed under air-tight state.
Aqua (AS) is to be dissolved in the water using certain raw medicines and Undec characteristic, is directly formulated with water Liquid.
Suspending agent (SC) refer to composition is mixed with suitable surfactant, water or organic solvent by a certain percentage, It is uniformly levigate through colloid mill, then grind 1 to 2 time through sand mill and be made to certain fineness.
Missible oil (EC), which refers to, to be dissolved composition in organic solvent by a certain percentage such as benzene,toluene,xylene, hexamethylene Ketone, and be added and prepare in the mixture of a certain amount of anion or nonionic surface active agent (emulsifier).
Microemulsion (ME) is generally made of liquid pesticide, surfactant (emulsifier), water, stabilizer etc.;Its main feature is that Using water as medium, be free of or less containing organic solvent.Drop size in microemulsion is generally several nanometers to tens nanometers, and being less than can The a quarter of light-exposed wavelength.
Aqueous emulsion (EW) is insoluble in the raw medicine liquid of water or raw medicine is dissolved in organic solvent acquired solution not soluble in water point It dissipates in one of water formulations of pesticide.Aqueous emulsion is the liquid pesticidal raw medicine that will be mixed to prepare with organic solvent with 0.5-1.5 μm The preparation that is dispersed in water of droplet, appearance is milky milk shape liquid.
Ultra-low volume spray agent refers to the medical fluid being sprayed onto being denoted as on object, and with superfine droplet, extremely low dosage sprays, and is For a kind of special dosage form of ultra-low volume spray application.
Seed coat agent (SD) is mixed effective component and auxiliary agent are ground, can be coated on kind of a sublist directly or after dilution Face forms the protective film with some strength and permeability.
Fumicants (FU) is also known as smoke agent, is to mix effective component and inflammable substance etc., is burnt, make pesticide Smog grain or a kind of medicament directly pesticide dispersion at smog grain are condensed into after gasification.
About the meaning of various adjuvants, various preparations, due to the difference in statement, the difference on understanding will cause.It answers When understanding, various adjuvants disclosed in this field, preparation belong to the range that the present invention covers, such as " pesticidal preparations add Work technology ", Luo Yanping, Song Weiwei, Chemical Industry Press, 2015;" pesticidal preparations ", Wang Kaiyun, Chinese agriculture publishing house, 2009;" Preparation Forms of Modern Pesticide processing technology book series ", Liu Guangwen, Chemical Industry Press, 2018;" formulations of pesticide and preparation and Application method ", Tu Yuqin, Golden Shield publishing house, 2008;" Chinese pesticide ", Chinese pesticide industry association;Etc. described in that A bit.The preparation method of various preparations includes but is not limited to those of described in the invention.
Above-mentioned preparation can be prepared in a way known, such as by by reactive compound or active agent combinations It is mixed at least one additive.Suitable additive is all conventional pharmaceutical adjuncts, such as organic solvent, filler, molten Agent or diluent, solid carrier and filler, surfactant (such as adjuvant, emulsifier, dispersing agent, protective colloid, wetting agent And tackifier), dispersing agent and/or adhesive or fixative, preservative, dyestuff and pigment, defoaming agent, inorganic and organic thickening Agent, hydrophober can also add drier and UV stabilizer, gibberellin and water and other processing aids if appropriate.At every kind In the case of, according to preparation type to be prepared, it may be necessary to other procedure of processings, such as wet lapping, dry grinding or granulation.
Preparation of the invention can reach effect same as composition described above, and details are not described herein again.
The present invention provides some preferred preparations to form, specific as follows:
Preferably, when the preparation is suspending agent, the adjuvant includes water, dispersing agent, wetting agent, defoaming agent, thickening Agent, stabilizer, antifreezing agent and at least one of the preservatives;
The dispersing agent preferably includes at least one of non-induced by alkyl hydroxybenzene and polycarboxylic acid salt, preferably TERSPERSE The combination of 4894 and GY-D800, the mass content preferably 2~6% in the preparation;
The wetting agent is preferably GY-WS03, the mass content in the preparation preferably 3~5%;
The defoaming agent is preferably organosilicon, the mass content in the preparation preferably 0.5~1.5%;
The thickener is preferably xanthan gum, the mass content in the preparation preferably 0.1~0.3%;
The stabilizer is preferably aluminium-magnesium silicate, the mass content in the preparation preferably 0.2~0.4%;
The antifreezing agent is preferably propylene glycol, the mass content in the preparation preferably 4~5%;
The preservative is preferably sodium benzoate, the mass content in the preparation preferably 0.05~0.15%.
Preferably, when the preparation is water dispersible granules, the adjuvant includes dispersing agent, carrier, defoaming agent, disintegrating agent At least one of with stabilizer;
The dispersing agent is preferably at least one of lignin and ethylene oxide propylene oxide block copolymer, preferably two The combination of person, the mass content preferably 7~10% in the preparation;
The carrier is preferably at least one of kaolin and organobentonite;
The defoaming agent is preferably organosilicon, the mass content in the preparation preferably 0.1~0.3%;
The disintegrating agent is preferably ammonium sulfate, the mass content in the preparation preferably 4~6%;
The stabilizer is preferably aluminium-magnesium silicate, the mass content in the preparation preferably 0.3~0.6%.
Preferably, when the preparation is wettable powder, the adjuvant includes dispersing agent, stabilizer, defoaming agent, thickening At least one of agent and carrier;
The dispersing agent preferably includes at least one of lignin and naphthalene sulphonate, preferably combination, Mass content preferably 8~12% in the preparation;
The stabilizer is preferably aluminium-magnesium silicate, the mass content in the preparation preferably 0.3~0.6%;
The defoaming agent is preferably organic silicone, the mass content in the preparation preferably 0.2~0.4%;
The thickener is preferably ammonium sulfate, the mass content in the preparation preferably 3~5%;
The carrier is preferably kaolin.
Preferably, when the preparation is aqueous emulsion, the adjuvant includes organic solvent, antifreezing agent, emulsifier, stabilization Agent, defoaming agent and water;
The organic solvent preferably includes at least one of cyclohexanone and dimethylbenzene, the preferably mixing of the two, described Mass content preferably 15~20% in preparation;
The antifreezing agent is preferably ethylene glycol, the mass content in the preparation preferably 3~5%;
The emulsifier preferably includes at least one of castor oil polyoxyethylene ether and TERMUL 2507, in the system Mass content preferably 5~7% in agent;
The stabilizer is preferably aluminium-magnesium silicate, the mass content in the preparation preferably 0.1~0.3%;
The defoaming agent is preferably organosilicon, the mass content in the preparation preferably 0.05~0.15%.
The above preferred preparation type composition, which can improve, improves medicament physicochemical property, such as stability, uniformity, quick-acting Or slow release etc., moreover it is possible to improve control efficiency.
In practical application, composition or preparation of the invention can handle all plant and plant part.Plant refers to All plants and plant population, such as want (whether to be planted with undesired wild plant, cultivar and plant variety The protection of article kind power or plant breeding power).Cultivar and plant variety can be (to be passed through by Sterile culture and breeding method One or more biotechnology methods are assisted or are supplemented, such as by using dihaploid, protoplast fusion, random mutagenesis With directed mutagenesis, molecular labeling or genetic marker), or the plant obtained by bioengineering and the method for genetic engineering.Plant Part refers to plant all part and organs above and below the ground, wherein list such as bud, leaf, Hua Hegen, such as leaf, needle, stem, Branch, flower, fructification, fruit and seed and root, bulb and rhizome.Crop and asexual and case of propagation material, such as cutting, Bulb, rhizome divide bark of a cork tree and seed to also belong to plant part.
For the present invention, term " effective quantity " refers to each active group for being enough to show desired control efficiency in dosage The total amount divided.This amount depends on the chemical combination for including in fungi, floristics, weather conditions and the present composition to be controlled Object and change in a wide range.
Conventional treatment side can be used to the processing that plant and plant part carry out with composition provided by the invention or preparation Method directly carries out or acts on its ambient enviroment, habitat or storage ground, for example, by dipping, sprinkling, be sprayed, irrigate, evaporate, spread Powder atomizing, broadcasts sowing, foams, smearing, being coated with, watering (pouring), instiling, and in the case of propagation materials, especially planting In the case where son, can also by involucrum (incrust), be coated with one or more layers coating etc. with powder-processed dry seeds, with solution It handles seed, slurries is handled with water-soluble powder.Composition or preparation can be also applied in soil.
It in the plant that can be protected by the method for the invention, can be mentioned that staple crops, be typically include Cereal At least one of crop, melon fruits and vegetables, such as corn and soybean, cotton, rape, rice, wheat, beet, sugarcane, oat, rye, big Wheat, grain, triticale, flax, liana and various fruit and vegetables from various plant classification groups, gardening and forest make Object;Ornamental plant;And the homologue of the genetic modification of these crops.
The present invention also includes the method for handling seed.Composition or preparation of the invention can be applied directly, i.e., do not include Other components and without dilution.Generally, it is preferred to which the present composition is applied to seed with suitable dosage form.
According to plant species or plant cultivars, their position and growth conditions (soil, weather, trophophase, nutrition), Processing of the invention can also bring superadditivity (" collaboration ") effect.Thus, for example, the following effect more than actual desired can be brought Fruit: the rate of application of the composition comprising Ipflufenoquin and olefin conversion that can be used according to the invention reduces and/or activity profile It widens and/or active increases, better plant growth, improves the tolerance to high temperature or low temperature, improves to arid or water or soil The tolerance of earth salt content improves Flowering quality, is easier harvesting, hasting of maturity, higher harvesting yield, bigger fruit Real, higher plant height, greener leaf color, make to bloom earlier, the quality of harvested products is higher and/or nutritive value more Sugared concentration high, in fruit is higher, harvested products storage stabilities and/or processability are more preferable.
Composition and preparation of the invention has significant control efficiency to fungus-caused plant related disease is prevented and treated, typically It is fallen including gray mold, head blight, banded sclerotial blight, powdery mildew, scab, spot, at least one of rust, leaf spot or target spot, It can be used for following typical plant: at least one of cereal crop, melon fruits and vegetables.
To sum up, compared with prior art, invention achieves following technical effects:
(1) it combines olefin conversion with Ipflufenoquin the synergistic effect that plays, and there is certain quick-acting And long-term effect;
(2) generation for delaying drug resistance improves the safety to crop;
(3) dosage is reduced, is reduced costs and manpower consumption;
(4) fungicidal spectrum is expanded.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products either obtained by commercially available purchase can be prepared by the method that the prior art is recorded.
Indoor biometrics experiment
Mycelial growth rate method is used indoors, measures different agents to wheat powdery mildew (Blumeria graminis) The inhibiting effect of growth calculates each medicament to the EC of pathogen50Value.
Activated spawn
(purchase is placed in picking strain from Chinese agriculture Microbiological Culture Collection administrative center, ACCC36953) from test tube Among potato dextrose agar (PDA) culture medium, after being placed in 26 DEG C of incubator culture 2d, then the picking bacterium from the bacterium colony of culture Kind, it is placed among new PDA culture medium, is placed in 26 DEG C of incubator culture 2d.
The weighing of sample is prepared
A certain amount of single dose or a certain proportion of composition (being shown in Table 1) are weighed, after solvent dmso solution, is added Containing 0.1% Tween 80-sterile water, it is made into certain density solution after mixing, then be diluted to 2mg/ by half dilution method L, each 5mL of the solution of the concentration gradient of 1mg/L, 0.5mg/L, 0.25mg/L, 0.125mg/L and 0.0625mg/L, it is spare.
Plate addition method
Toxic plate is made using compound and culture medium: in superclean bench, (being cooled to 45mL PDA culture medium 45-50 DEG C) in sterilized compound solution 5mL (sterilization method: ultraviolet sterilization) is added, be uniformly mixed, pour into plate (diameter 90mm), cooling, repeat 3 plates.The PDA of compound solution is replaced to train so that the sterile water of equivalent emulsifier containing same solvent is added Base is supported as blank control.
Picking inoculation fungus block (diameter 6mm) is put upside down in plate center, and 2d (incubation time is cultivated in 26 DEG C of constant incubators It should be depending on growing state, when generally colony diameter grows to 70-80mm in blank control).It is measured with crossing method Colony diameter.
Bacterium colony extends diameter (mm)=bacterium colony average diameter (mm) -6 (mm)
Biometrics probability value are tabled look-up according to relative inhibition and can be obtained.Using log concentration as abscissa, according to " biology is united Count probit value conversion table ", inhibition percentage is converted into biological probability value as ordinate, draws virulence regression equation.It utilizes The mass concentration that equation acquires when probability value are 5 is EC50(Millot M,Girardot M,Dutreix L,et al..Antifungal and anti-biofilm activities of acetone lichen extracts against Candida albicans.[J].Molecules,2017,22(4):651.)。
Using the co-toxicity coefficient method of the abundant calculating of Sun Yun, the co-toxicity coefficient (CTC) of mixture is calculated, determines the synergy of mixture Property.
Using single dose a certain in mixture as standard agent, calculated:
The single dose toxicity index=(EC of standard agent50/ certain single dose EC50)×100
Theoretical toxicity index (TTI)=A single dose toxicity index × A single dose proportion+B single dose in mixture virulence Index × B single dose proportion in mixture
Survey toxicity index (ATI)=(EC of standard single dose50Value/mixture EC50Value) × 100
Co-toxicity coefficient=(survey toxicity index/theoretical toxicity index) × 100
Mixture has synergetic (the simple adduction compared with its single dose is significantly increased) when CTC is greater than 120, and CTC is small It is antagonism when 80, CTC is summation action between 80-120.
Table 1: the measurement knot of olefin conversion and Ipflufenoquin different ratio (mass ratio) to wheat powdery mildew co-toxicity coefficient Fruit
Conclusion: as can be seen from Table 1, using Ipflufenoquin and olefin conversion as effective component in the embodiment of the present invention, It is significant to wheat powdery mildew control efficiency when forming composition with above-mentioned different quality ratio.Wherein, olefin conversion with Ipflufenoquin is when mass ratio is between (1:1)~(1:15), i.e. content >=olefin conversion of Ipflufenoquin When content, co-toxicity coefficient is greater than 120, has obvious synergistic function.As it can be seen that the group of Ipflufenoquin and olefin conversion The favourable agents of prevention and treatment wheat powdery mildew can be become by closing object.
The Ipflufenoquin of embodiment 1 30% and the suspending agent of olefin conversion
1. crushing the preparation of slurry
Disperse non-induced by alkyl hydroxybenzene dispersant with high efficiency (trade name: TERSPERSE 4894, Huntsman) in 42g water High-molecular compound dispersing agent (trade name: GY-800, Beijing Guang Yuan benefit agriculture) 1.2g, wetting agent (commodity of 1.8g, comb-type structure Name: GY-WS03, Beijing Guang Yuan benefit agriculture) 4g and silicone antifoaming agent (Hangzhou Zuo Tu new material Co., Ltd) 1g, wherein Disperse Ipflufenoquin raw medicine 15g, the raw medicine 15g of olefin conversion, usesBead is carried out wet with sand mill Method crushes 2.0h, obtains and crushes slurry 80g.
2. the modulation of decentralized medium
Disperse xanthan gum 0.2g, aluminium-magnesium silicate 0.3g, 1,2-PD 4.2g and sodium benzoate 0.1g in 15.2g water, Obtain decentralized medium 20g.
3. the modulation of aqueous suspension shape composition pesticide
Above-mentioned crushing slurry 80g and decentralized medium 20g are mixed, aqueous suspension shape composition pesticide 100g is obtained, (4000 revs/min) 30 minutes under high speed disperser high speed shear are made effective component (Ipflufenoquin and olefin conversion) The suspending agent that mass content is 30%.
The Ipflufenoquin of embodiment 2 40% and the suspending agent of olefin conversion
1. crushing the preparation of slurry
Disperse non-induced by alkyl hydroxybenzene dispersant with high efficiency (trade name: TERSPERSE 4894, Huntsman) in 32g water High-molecular compound dispersing agent (trade name: GY-D800, Beijing Guang Yuan benefit agriculture) 1.2g, wetting agent (quotient of 1.8g, comb-type structure The name of an article: GY-WS03, Beijing Guang Yuan benefit agriculture) 4g and silicone antifoaming agent (ETXP-40, the limited public affairs of the left native new material in Hangzhou Department) 1g, disperses Ipflufenoquin raw medicine 30g, the raw medicine 10g of olefin conversion wherein, usesBead (Zhejiang Jiang Jinkun Gao Ye Co., Ltd), wet pulverizing 2.0h is carried out with sand mill, obtains and crushes slurry 80g.
2. the modulation of decentralized medium
Disperse xanthan gum 0.2g, aluminium-magnesium silicate 0.3g, 1,2-PD 4.2g and sodium benzoate 0.1g in 15.2g water, Obtain decentralized medium 20g.
3. the modulation of aqueous suspension shape composition pesticide
Above-mentioned crushing slurry 80g and decentralized medium 20g are mixed, aqueous suspension shape composition pesticide 100g is obtained, (4000 revs/min) 30 minutes under high speed disperser high speed shear are made effective component (Ipflufenoquin and olefin conversion) The suspending agent that mass content is 40%.
The Ipflufenoquin of embodiment 3 50% and the water dispersible granules of olefin conversion
By raw medicine 25g, the EOPO block copolymer (trade name: Antraox of Ipflufenoquin raw medicine 25g, olefin conversion B/848, Luo Diya) it is 5g, lignin (trade name: WG4, Shanghai outstanding person's generation chemical industry) 3g, ammonium sulfate 5g, aluminium-magnesium silicate 0.5g, organic Bentonite 0.2g, silicone antifoaming agent (Hangzhou Zuo Tu new material Co., Ltd) 0.2g mixing, add to 100g with kaolin, First precomminution mixes, then is granulated through air-flow crushing to required partial size, again using rotating pelletizer, and effective component is made The water dispersible granules that (Ipflufenoquin and olefin conversion) mass content is 50%.
The Ipflufenoquin of embodiment 4 60% and the water dispersible granules of olefin conversion
By raw medicine 10g, the EOPO block copolymer (trade name: Antraox of Ipflufenoquin raw medicine 50g, olefin conversion B/848, Luo Diya) it is 5g, lignin (trade name: WG4, Shanghai outstanding person's generation chemical industry) 3g, ammonium sulfate 5g, aluminium-magnesium silicate 0.5g, organic Bentonite 0.2g, silicone antifoaming agent (Hangzhou Zuo Tu new material Co., Ltd) 0.2g mixing, add to 100g with kaolin, First precomminution mixes, then is granulated through air-flow crushing to required partial size, again using rotating pelletizer, and effective component is made The water dispersible granules that (Ipflufenoquin and olefin conversion) mass content is 60%.
The Ipflufenoquin of embodiment 5 60% and the wettable powder of olefin conversion
By Ipflufenoquin raw medicine 45g, the raw medicine 15g of olefin conversion, naphthalene sulphonate (trade name: Morwet D-425, Akzo Nobel) 6g, lignin (trade name: WG4, Shanghai outstanding person's generation chemical industry) 4g, ammonium sulfate 4g, aluminium-magnesium silicate 0.5g, organic silicone (trade name: DOW CORNING ANTIFOAM C EMULSION, DOW CORNING) 0.3g mixing, are used Kaolin adds to 100g, and first precomminution mixes, then through air-flow crushing to required partial size, effective component (Ipflufenoquin is made And olefin conversion) mass content be 60% wettable powder.
The Ipflufenoquin of embodiment 6 30% and the aqueous emulsion of olefin conversion
1. oily mutually prepare
The mixing that Ipflufenoquin raw medicine 15g, olefin conversion raw medicine 15g are added to cyclohexanone 10g and dimethylbenzene 7g is molten In agent, after ultrasonic mixing is uniform, then by emulsifier (trade name: TERMUL 2507, Huntsman) 2g, castor oil polyoxy Vinethene (trade name: EMULPON CO-360, Akzo Nobel) 4g is added and is slowly stirred to being completely dissolved.
2. prepared by water phase
By ethylene glycol 4g, aluminium-magnesium silicate 0.2g, silicone antifoaming agent (Hangzhou Zuo Tu new material Co., Ltd) 0.1g Mixing, adds water 42.7g to stir evenly.
3. composition pesticide aqueous emulsion is deployed
Water phase is slowly added in oily phase, and is stirred continuously until after being added completely under high speed disperser high speed shear The water and milk that effective component (Ipflufenoquin and olefin conversion) mass content is 30% is made in (4000 revs/min) 30 minutes Agent.
The Ipflufenoquin water dispersible granules of reference examples 1 30%
By Ipflufenoquin raw medicine 30g, naphthalene sulphonate (trade name: Morwet D-425, Aksu promise shellfish You) 6g, lignin (trade name: WG4, Shanghai outstanding person's generation chemical industry) 4g, ammonium sulfate 4g, aluminium-magnesium silicate 0.5g, organic silicone (commodity Name: DOW CORNING ANTIFOAM C EMULSION, DOW CORNING) 0.3g mixing, 100g is added to kaolin, it is first pre- It crushes and mixes, then through air-flow crushing to required partial size, the water that effective component (Ipflufenoquin) mass content is 30% is made Dispersible granule.
The diniconazole suspending agent of reference examples 2 20%
1. crushing the preparation of slurry
Bonus point dissipates non-induced by alkyl hydroxybenzene dispersant with high efficiency (trade name: TERSPERSE 4894, Huntsman) in 52.6g water High-molecular compound dispersing agent (trade name: GY-900, Beijing Guang Yuan benefit agriculture) 1.6g, wetting agent (commodity of 1.4g, comb-type structure Name: GY-WS10, Beijing Guang Yuan benefit agriculture) 4g and silicone antifoaming agent (Hangzhou Zuo Tu new material Co., Ltd) 0.4g, at it Middle dispersion olefin conversion raw medicine 20.0g is usedBead uses sand mill
Wet pulverizing 1.5h is carried out, obtains and crushes slurry 80g.
2. the modulation of decentralized medium
Disperse xanthan gum 0.3g, aluminium-magnesium silicate 0.4g, ethylene glycol 4g and sodium benzoate 0.1g in water 15.2g, is divided Dispersion media 20g.
3. the modulation of aqueous suspension shape composition pesticide
Above-mentioned crushing slurry 80g and decentralized medium 20g are mixed, aqueous suspension shape composition pesticide 100g is obtained, (4000 revs/min) 30 minutes under high speed disperser high speed shear, it is 20% that effective component (olefin conversion) mass content, which is made, Suspending agent.
Reference examples 3
100g blank clear water.
Field control effectiveness test
Test process: according to the reagent agent experimental design in table 2, three are set separately to the test medicine of embodiment 1-6 A effective ingredient consumption.Comparison medicament is respectively reference examples 1, reference examples 2 and reference examples 3.
Table 2: reagent agent experimental design
Cell setting: each plot area is 66.7m2
Application method: being administered in wheat powdery mildew early growth period, and foliar spray processing, spouting liquid is based on drop of not dripping;
Spraying times: 3 times, such as strong wind weather or it is expected that rainfall in 1 hour, then be not administered.Investigation disease before application for the first time Feelings radix was administered every 7 days 1 time, 7 days investigation preventive effects after the 3rd application later.
Control time and number: progress radix investigation in 1 day after application, 7 days, 14 days, 21 days progress wheat powdery mildews after medicine Growing state investigation.
Investigation method: according to wheat powdery mildew upgrowth situation, as unit of strain, 5 points of every cell diagonal line samplings, every point Investigation is connected 5 clumps, totally 25 clumps, records total strain number and growing state.
Inspection drug effect method after investigating and prevent and treat before application are as follows: 5 points of grab sample in test process area record total leaf Number, the sick number of sheets and sick series.Grade scale method is as follows:
0 grade: complete stool is disease-free;
1 grade: quaterfoil and its following leaf sheath, blade morbidity (with sword-like leave for first leaf);
3 grades: third blade and its following leaf sheath, blade morbidity;
5 grades: second blades and its following leaf sheath, blade morbidity;
7 grades: sword-like leave and its following leaf sheath, blade morbidity;
9 grades: complete stool morbidity, it is withered ahead of time.
Drug effect calculates:
See Table 3 for details for test result.
Table 3: preventive effect of the different agents to wheat powdery mildew
Conclusion: from table 3 it can be seen that white wheat after the Ipflufenoquin of the embodiment of the present invention and olefin conversion combination The control efficiency of powder disease is substantially better than comparison medicament, and two kinds of ingredients are combined in certain proportion, compared to exclusive use pair According to medicament, it can reach 80% or more within 7 days after medicine, improve quick-acting;Control efficiency at 21 days is 80% or more, holding effect Phase is extended, and has synergistic function.In addition, not finding the composition of the embodiment of the present application to wheat in scope of medication There is no phytotoxicity generation, shows that the bactericidal composition of the application is good to crop safety.
The foregoing is only a preferred embodiment of the present invention, but scope of protection of the present invention is not limited thereto, In the technical scope disclosed by the present invention, any changes or substitutions that can be easily thought of by anyone skilled in the art, It should be covered by the protection scope of the present invention.Therefore, protection scope of the present invention should be with the protection model of the claim Subject to enclosing.

Claims (12)

1. a kind of composition, which is characterized in that including drug activity component;
The drug activity component includes active constituent a and active constituent b, and the active constituent a is olefin conversion, the activity at Dividing b is Ipflufenoquin.
2. composition according to claim 1, which is characterized in that the quality of the active constituent a and the active constituent b Than being 1~30: 30~1, preferably 1~15: 15~1, more preferable 1: 1~15, still more preferably 1: 1~5;Or preferably 1~5:5 ~1;
Preferably, in the composition, the content of the active constituent a≤active constituent b content.
3. composition according to claim 1, which is characterized in that the total content of the drug activity component in the composition For 1~95wt.%, preferably 20~80wt.%, more preferable 30~60wt.%.
4. composition according to claim 1-3, which is characterized in that it further include adjuvant, the adjuvant packet Include wetting agent, dispersing agent, emulsifier, thickener, disintegrating agent, antifreezing agent, defoaming agent, solvent, preservative, stabilizer, synergist At least one of with carrier.
5. the preparation of the described in any item composition preparations of claim 1-4, which is characterized in that the type of the preparation is cream Oil, wettable powder, suspending agent, granule, water dispersion granule, microemulsion, aqueous emulsion, microcapsule formulations, spray, seed coat agent Or fumicants.
6. preparation according to claim 5, which is characterized in that the preparation be suspending agent when, the adjuvant include water, Dispersing agent, wetting agent, defoaming agent, thickener, stabilizer, antifreezing agent and at least one of the preservatives;
The dispersing agent preferably includes at least one of non-induced by alkyl hydroxybenzene and polycarboxylic acid salt;
The wetting agent is preferably GY-WS03;
The defoaming agent is preferably organosilicon;
The thickener is preferably xanthan gum;
The stabilizer is preferably aluminium-magnesium silicate;
The antifreezing agent is preferably propylene glycol;
The preservative is preferably sodium benzoate.
7. preparation according to claim 5, which is characterized in that when the preparation is water dispersible granules, the adjuvant packet Include at least one of dispersing agent, carrier, defoaming agent, disintegrating agent and stabilizer;
The dispersing agent is preferably at least one of lignin and ethylene oxide propylene oxide block copolymer;
The carrier is preferably at least one of kaolin and organobentonite;
The defoaming agent is preferably organosilicon;
The disintegrating agent is preferably ammonium sulfate;
The stabilizer is preferably aluminium-magnesium silicate.
8. preparation according to claim 5, which is characterized in that when the preparation is wettable powder, the adjuvant packet Include at least one of dispersing agent, stabilizer, defoaming agent, thickener and carrier;
The dispersing agent preferably includes at least one of lignin and naphthalene sulphonate;
The stabilizer is preferably aluminium-magnesium silicate;
The defoaming agent is preferably organic silicone;
The thickener is preferably ammonium sulfate;
The carrier is preferably kaolin.
9. preparation according to claim 5, which is characterized in that when the preparation is aqueous emulsion, the adjuvant includes Solvent, antifreezing agent, emulsifier, stabilizer, defoaming agent and water;
The organic solvent preferably includes at least one of cyclohexanone and dimethylbenzene;
The antifreezing agent is preferably ethylene glycol;
The emulsifier preferably includes at least one of castor oil polyoxyethylene ether and TERMUL 2507;
The stabilizer is preferably aluminium-magnesium silicate;
The defoaming agent is preferably organosilicon.
10. the described in any item compositions of claim 1-4 or the described in any item preparations of claim 5-9 draw in prevention and treatment fungi The application in plant related disease risen;
Preferably, the related disease include gray mold, head blight, banded sclerotial blight, powdery mildew, scab, spot fall, rust, leaf At least one of pinta or target spot;
Preferably, the plant includes being selected from least one of cereal crop, melon fruits and vegetables.
11. the method for preparing composition described in any one of claim 1-4, the method includes by olefin conversion and Ipflufenoquin is combined.
12. the method for preparing preparation described in any one of claim 5-9, the method includes by olefin conversion and Ipflufenoquin is in conjunction with one or more adjuvants.
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