CN106465717B - A kind of Synergistic herbicide compositions - Google Patents

A kind of Synergistic herbicide compositions Download PDF

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Publication number
CN106465717B
CN106465717B CN201510821143.3A CN201510821143A CN106465717B CN 106465717 B CN106465717 B CN 106465717B CN 201510821143 A CN201510821143 A CN 201510821143A CN 106465717 B CN106465717 B CN 106465717B
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herbicidal combinations
combinations according
active components
active constituent
active
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CN106465717A (en
Inventor
金涛
王金信
路兴涛
彭学岗
张景远
赵德
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Qingdao Qingyuan Resistance Weed Prevention And Treatment Co Ltd
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Qingdao Qingyuan Resistance Weed Prevention And Treatment Co Ltd
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    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/48—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with two nitrogen atoms as the only ring hetero atoms
    • A01N43/56—1,2-Diazoles; Hydrogenated 1,2-diazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N35/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical
    • A01N35/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical at least one of the bonds to hetero atoms is to nitrogen
    • A01N35/10—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom having two bonds to hetero atoms with at the most one bond to halogen, e.g. aldehyde radical at least one of the bonds to hetero atoms is to nitrogen containing a carbon-to-nitrogen double bond
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/34—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with one nitrogen atom as the only ring hetero atom
    • A01N43/40—Biocides, 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
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/66—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms
    • A01N43/68—1,3,5-Triazines, not hydrogenated and not substituted at the ring nitrogen atoms with two or three nitrogen atoms directly attached to ring carbon atoms
    • A01N43/70—Diamino—1,3,5—triazines with only one oxygen, sulfur or halogen atom or only one cyano, thiocyano (—SCN), cyanato (—OCN) or azido (—N3) group directly attached to a ring carbon atom
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/64—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with three nitrogen atoms as the only ring hetero atoms
    • A01N43/707—1,2,3- or 1,2,4-triazines; Hydrogenated 1,2,3- or 1,2,4-triazines
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/72—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms
    • A01N43/74—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having rings with nitrogen atoms and oxygen or sulfur atoms as ring hetero atoms five-membered rings with one nitrogen atom and either one oxygen atom or one sulfur atom in positions 1,3
    • A01N43/76—1,3-Oxazoles; Hydrogenated 1,3-oxazoles
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N43/00—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds
    • A01N43/90—Biocides, pest repellants or attractants, or plant growth regulators containing heterocyclic compounds having two or more relevant hetero rings, condensed among themselves or with a common carbocyclic ring system
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/30—Derivatives containing the group >N—CO—N aryl or >N—CS—N—aryl
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/36—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< directly attached to at least one heterocyclic ring; Thio analogues thereof
    • A—HUMAN NECESSITIES
    • A01—AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01N—PRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N47/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid
    • A01N47/08—Biocides, pest repellants or attractants, or plant growth regulators containing organic compounds containing a carbon atom not being member of a ring and having no bond to a carbon or hydrogen atom, e.g. derivatives of carbonic acid the carbon atom having one or more single bonds to nitrogen atoms
    • A01N47/28—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N<
    • A01N47/38—Ureas or thioureas containing the groups >N—CO—N< or >N—CS—N< containing the group >N—CO—N< where at least one nitrogen atom is part of a heterocyclic ring; Thio analogues thereof

Abstract

The invention belongs to pesticide synergistic technical fields, and in particular to one kind includes the Synergistic herbicide compositions of 1- (the chloro- 3- of 2- (3- cyclopropyl -5- hydroxyl -1- methyl-1 H- pyrazoles -4- carbonyl) -6- trifluoromethyl) piperidines -2- ketone.The Synergistic herbicide compositions include the active components A and active constituent B of herbicidally effective amount, wherein active components A is compound

Description

A kind of Synergistic herbicide compositions
Technical field
The invention belongs to pesticide synergistic technical fields, and in particular to one kind includes 1- (the chloro- 3- of 2- (3- cyclopropyl -5- hydroxyl Base -1- methyl-1 H- pyrazoles -4- carbonyl) -6- trifluoromethyl) piperidines -2- ketone Synergistic herbicide compositions.
Background technique
It is means the most economical and effective during farmland weed is prevented and kill off using herbicide chemical weed control.But long-term continuous high agent The problems such as amount ground uses the chemical herbicide of single variety or the single mode of action, be easy to cause weeds drug resistance and resistance evolution. The reasonable compounding or mixture of herbicidal compounds, which have, to be expanded weeds spectrum, improves preventive effect, delays weeds drug resistance and anti-medicine The advantages that generation and development of property, be one of the most effective methods to solve the above problems.
P _ Hydroxyphenyl pyruvic acid dual oxide enzyme (HPPD) is after acetyl-CoA carboxylase (ACCase) inhibitor, acetyl cream The another class novel herbicidal found after acid enzyme (ALS) inhibitor and proporphyrinogen oxidase (Protox) inhibitor etc. Agent.The action character of HPPD inhibitor is the activity of weeding with wide spectrum, be can be used before bud and after bud, after albefaction occur in weeds It is dead.Though its symptom and the effect symptom of carotenoid biostatic agent are extremely similar, its chemical structure feature such as polarity and electricity There is apparent difference with known carotenoid biostatic agent from degree.HPPD inhibitor class herbicide Weed Resistance risk is big Be lower than ACCase inhibitor and ALS inhibitor greatly, and with the wheats such as fenoxapropPethyl, clodinafop-propargyl, pinoxaden, tralkoxydim ALS inhibitor is often often used with the wheat paddocks such as ACC inhibitor and flucarbazone, mesosulfuron, pyroxsulam in field, and there is no targets Cross resistance caused by resistance.
Photosynthesis Photosystem I I herbicide, phytoene dehydrogenase (PDS) inhibitor class herbicide are in wheat paddock Weeds chemoprevention system occupies critical positions.
The common photosynthesis Photosystem I I herbicide of wheat paddock has: isoproturon, chlortoluron, terbutryn, prometryn, piperazine grass Ketone etc.；Photosynthesis Photosystem I I herbicide is cauline leaf process contact killing type herbicide after electing property bud, is mainly absorbed by blade, By inhibiting photosynthetic each process, make tissue necrosis rapidly.The above medicament can be used for wheat paddock and prevent and kill off amur foxtail, Japan The raw gramineae weeds such as amur foxtail, Wang grass, hard grass, wild avena sativa, Itanlian rye, but when such medicament is applied alone, dosage is more, and To wheat, there are heavier security risks, and dosage is poor to the preventive effect of weeds when few, need strictly to hold pesticide application technology and apply Pharmaceutical quantities.The wheat paddocks such as photosynthesis Photosystem I I herbicide and fenoxapropPethyl, clodinafop-propargyl, pinoxaden, tralkoxydim are normal Often using ALS inhibitor with the wheat paddocks such as ACC inhibitor and flucarbazone, mesosulfuron, pyroxsulam, there is no target resistances Caused cross resistance.
The common phytoene dehydrogenase inhibitor class herbicide of wheat paddock has: diflufenican, fluorine pyrrole acyl grass amine Deng the medicine belongs to herxheimer-liked reaction inhibitor, leads to Destruction of Chlorophyll and cell rupture, Plant death, is wide spectrum Selective cornfield herbicidal prevents and kill off amur foxtail, Alopecurus, Wang grass, hard grass, wild avena sativa, more suitable for barley, wheat paddock The raw gramineae weeds such as flower rye grass.But such medicament, when being applied alone, dosage is more, and there are heavier safety wind to wheat Danger, dosage is poor to the preventive effect of weeds when few, needs strictly to hold pesticide application technology and application dosage.Phytoene dehydrogenase The wheat paddocks such as inhibitor class herbicide and fenoxapropPethyl, clodinafop-propargyl, pinoxaden, tralkoxydim often use ACC inhibitor and fluorine The wheat paddocks such as azoles sulphur is grand, mesosulfuron, pyroxsulam often use ALS inhibitor, and there is no cross resistances caused by target resistance.
Summary of the invention
To solve the above-mentioned problems in the prior art, the present invention provides a kind of comprising 1- (2- chloro- 3- (3- cyclopropyl- 5- hydroxyl -1- methyl-1 H- pyrazoles -4- carbonyl) -6- trifluoromethyl) piperidines -2- ketone Synergistic herbicide compositions, the combination Object can effectively prevent and kill off the gramineae weed in wheat paddock, have obvious expansion degrass spectrum, synergistic effect, reduction amount of application, to work The features such as object is safe.
A kind of Synergistic herbicide compositions comprising the active components A and active constituent B of herbicidally effective amount, wherein
Active components A is compound
Active constituent B can be selected from one of following compound or a variety of:
1) ureas: isoproturon, chlortoluron；
2) pyridines: diflufenican, fluorine pyrrole acyl grass amine；
3) aryloxyphenoxypropionate class: fenoxapropPethyl, clodinafop-propargyl, alkynes oxalic acid；
4) cyclohexyl diketone: tralkoxydim；
5) sulfonylurea: mesosulfuron, Sulfosulfuron, procarbazone, flucarbazone；
6) triazines: metribuzin, prometryn, terbutryn；
7) sulfonamides: pyroxsulam；
8) phenylpyrrazolin class: pinoxaden.
Preferably, the active constituent B is isoproturon, chlortoluron, diflufenican, fluorine pyrrole acyl grass amine, smart oxazole Diclofop-methyl, clodinafop-propargyl, alkynes oxalic acid, tralkoxydim, mesosulfuron, flucarbazone, metribuzin, prometryn, terbutryn, pyridine sulphur grass One of amine, pinoxaden are a variety of.
Wherein, it is 1-80:1-80,1-50:1-50 that the weight ratio of A and B, which is the weight ratio of 1-100:1-100, preferably A and B, The weight ratio of 1-30:1-30, more preferable A and B are 1-20:1-20,1-10:1-10, living defined by the range of weight ratio Property ingredient A and active constituent B mixture obtain synergistic technical effect.
The mass percentage of A and B accounts for the 1-95% of total amount, preferably 10-80% in the Synergistic herbicide compositions.It is logical Often, Herbicidal combinations of the invention include the active constituent of 1-95 parts by weight and the pesticide conven-tional adjuvants of 5-99 parts by weight.
The conven-tional adjuvants of the present composition can be carrier, surfactant etc..
Term " carrier " herein indicates a kind of organic or inorganic, natural or synthetic substance.They facilitate activity The application of ingredient, the carrier be usually it is inert and must be it is agriculturally acceptable, especially processed plant is received. Carrier can be solid, such as clay, natural or synthetic silicate, silica, resin, wax, solid fertilizer；Or liquid Body, such as water, alcohols, ketone, petroleum distillate, aromatic hydrocarbons or wax hydrocarbon, chlorohydrocarbon, liquefied gas.
Surfactant may include emulsifier, dispersing agent or wetting agent, it can be ionic or non-ionic.It can mention And example be the salt of polyacrylic acid, lignosulfonates, phenolsulfonic acid or naphthalene sulfonic acids salt, ethylene oxide and aliphatic alcohol or Polymer, sulfosuccinic acid with aliphatic acid or with aliphatic amine and fortified phenol (especially alkylphenol or aryl phenol) Phosphate, the alkyl of the phenol of salt, taurine derivatives (especially taurine alkane rouge) and alcohol phosphate or multi-hydroxy ethyl Sulfonate, alkylaryl sulfonates, alkyl sulfate, lauryl ether sulfate, aliphatic alcohol sulfate and sulphation 16-, 17-and octadecanol and sulphated fatty alcohol glycol ether, in addition there are the condensations of naphthalene or naphthalene sulfonic acids and phenol and formaldehyde Object, NONIN HS 240, ethoxylated isooctyl-phenol, octyl phenol or nonyl phenol, alkyl phenyl polyglycol ether, three fourths Base phenyl polyglycol ether, three stearyl phenyl polyglycol ethers, alkyl aryl polyether alcohol, pure and mild fatty alcohol/ethylene oxide contracting Close object, ethoxylated castor oil, polyoxyethylene alkyl ether, ethoxylation polyoxypropylene, laruyl alcohol polyglycol ether acetal, sorb Alcohol ester, lignin sulfite waste liquor and protein, albuminate, polysaccharide (such as methylcellulose), Hydrophobic Modified Starch, Polyvinyl alcohol, polycarboxylate, poly-alkoxyl compound, polyvinylamine, polyvinylpyrrolidone and its copolymer.At least need one kind Surfactant exists, to be conducive to active constituent dispersion in water and be conducive to enable them to correctly be applied to plant.
Above-mentioned composition contains various other components, such as protecting colloid, adhesive, thickener, thixotropic agent, infiltration Agent, stabilizer, chelating agent, dyestuff, colorant and polymer.
Composition of the invention can used before through dilution or directly by user.It, which is prepared, to be added by common Work method preparation, i.e., after active material being mixed with liquid solvent or solid carrier, add surfactant such as dispersing agent, surely Determine one or more of agent, wetting agent, adhesive, defoaming agent etc..
The specific preparation of the Herbicidal combinations is missible oil, suspending agent, microemulsion, suspoemulsion, aqueous emulsion, oily hang can be dispersed Floating agent, wettable powder or water dispersible granules (dry suspending agent).
Comprising following constituent content when wettable powder is made in composition: active components A 1~70%, active constituent B 1 ~50%, dispersing agent 5~10%, wetting agent 2~10%, filler surplus.
Active components A, active constituent B, dispersing agent, wetting agent, filler are mixed, are uniformly mixed in mixed cylinder, through gas Stream pulverizer remixes uniformly after crushing, that is, can be made into the wettable powder product of the present composition.
Composition includes following constituent content when water dispersible granules are made: active components A 1~70%, active constituent B 1 ~50%, dispersing agent 3~12%, wetting agent 1~8%, disintegrating agent 1~10%, binder 1~8%, filler surplus.
Active components A, active constituent B, dispersing agent, wetting agent, disintegrating agent, filler etc. are needed through air-flow crushing together The partial size wanted adds other auxiliary agents such as binder, obtains granulation materials.Item is quantified and is sent into fluidized bed granulating dryer After granulation and drying, the water dispersible granules product of the present composition is made.
Composition includes following constituent content when suspending agent is made: active components A 0.1~40%, active constituent B 0.1 ~30%, dispersing agent 2~10%, wetting agent 2~10%, defoaming agent 0.1~1%, binder 0.1~2%, antifreeze 0.1~ 8%, deionized water adds to 100%.
Dispersing agent, wetting agent, defoaming agent, thickener, antifreeze in above-mentioned formulation material are uniformly mixed by high speed shear, Active components A, active constituent B is added, in the ball mill ball milling 2~3 hours, makes diameter of particle all at 5 μm hereinafter, this is made The suspending agent product of inventive composition.
Composition includes following constituent content when suspoemulsion is made: active components A 0.1~40%, active constituent B 0.1 ~30%, emulsifier 2~12%, dispersing agent 2~10%, defoaming agent 0.1~2%, thickener 0.1~2%, antifreeze 0.1~ 8%, stabilizer 0.05~3%, water add to 100%.
Dispersing agent, defoaming agent, thickener, antifreeze, stabilizer in above-mentioned formulation material are uniformly mixed by high speed shear, Active constituent B raw medicine is added, in the ball mill ball milling 2~3 hours, makes diameter of particle all at 5 μm hereinafter, active constituent is made Then B suspending agent directly emulsifies active components A raw medicine, emulsifier and various auxiliary agents into suspending agent with high speed agitator, system Obtain the suspoemulsion product of the present composition.
Composition includes following constituent content when aqueous emulsion is made: active components A 0.1%~40%, active constituent B 0.1%~30%, solvent 2%~10%, emulsifier 2%~12%, dispersing agent 2%~10%, co-emulsifier 0.2%~5%, Antifreeze 0.1%~8%, defoaming agent 0.1%~2%, thickener 0.1%~2%, deionized water add to 100%.
To there are raw medicine, solvent, emulsifier, co-emulsifier to be added together in above-mentioned formula, makes to be dissolved into homogeneous oil phase.It will go Ionized water, dispersing agent, antifreeze, defoaming agent, thickener mix, under high velocity agitation, water phase is slow at uniform water phase It is slow to instill oily phase, the well dispersed aqueous emulsion product of the present composition is made.
Composition includes following constituent content when microemulsion is made: active components A 0.1%~40%, active constituent B 0.1%~30%, emulsifier 5%~15%, solvent 2%~10%, antifreeze 5%~10%, stabilizer 0.5%~3%, go Ionized water adds to 100%.
Raw medicine in above-mentioned formula, solvent, emulsifier are added in mother liquor modulation kettle, homogeneous oil phase is made, by deionized water, In the uniformly mixed injection product modulation kettle such as antifreeze, through high-speed stirred, it is uniformly mixed that the present composition is made is transparent or half Transparent microemulsion product.
In brief, composition of the invention can be added with conventional use of solid in the formula of the prior art and liquid Agent mixing.
In further preferred form of implementation, the Herbicidal combinations further include safener C, selected from pyrazoles solution grass Ester, cloquintocetmexyl, isoxadifen, cyclopropyl-sulfonylamide, naphthalic anhydride (NA), chlorine oxalene peace, R-28725, AD-67, CGA- 154281(Benoxacor)、CGA-43089(Cyometrinil)、CGA-43089(Cyometrinil)、Hoe-70542 (Fenchlorazole), benoxacor (Fenclorim), flurazole, BAS-145138, MON-13900, quinoline, sulphonyl Urea (amine) class safener, 2,4-D (organic acid), novel Antidote T (main ingredient 4%Ti4+) and gibberellin (GA) in one Kind is a variety of.
Composition of the invention can be applied on plant leaf blade to be processed by spraying method, that is, be applied to weeds, It is especially invaded and harassed on the harmful weed infestation of plant growth or easily on the surface of influence, the administration dosage of these active constituents is usual At 15-1500 grams/ha, preferably 30-750 grams/ha.
Herbicidal combinations of the present invention are shown in the 3 leaf phase of wheat by 2 years field control effectiveness tests to period of seedling establishment, miscellaneous The careless 1-5 leaf not equal phases, wheat has no symptom of chemical damage from application to the maturity period, to wheat safety.Preventive effect 45 days of weeds reach 90% or more, with the increase of dosage, preventive effect is obviously increased, and primary application can control miscellaneous in crop entire growth period Grass, not only herbicidal effect is significant, but also environmentally friendly, on second stubble crop without influence.
When applying Herbicidal combinations of the invention, unexpected synergistic effect is obtained, and activity of weeding ratio makes It is individually active more significant with the expected summation of the activity of single herbicide, and single herbicide.Synergistic effect shows as applying Measure reductions, broader weeds distribution spectrum, herbicide effect faster, it is more longlasting, these characteristics are required in Weeds distribution practice process It wants.For described characteristic, these new compositions are significantly superior to existing herbicide.
Herbicidal combinations of the invention also have advantages in that
(1) composition of the invention belongs to environmentally friendly herbicide, is easy to degrade in the environment, to when stubble wheat and Succession crop is very safe.
(2) Herbicidal combinations of the present invention are at low cost, easy to use, and popularization and application have huge economic benefit and society's effect Benefit.
(3) compared with prior art, Herbicidal combinations of the present invention can prevent and kill off non-resistance gramineae weed and prevent It is the effective scheme of weeds of wheat resistance management except the gramineae weed for generating resistance to ALS and ACC inhibitor.
Specific embodiment
The following example not limits the present invention, and is used only to illustrate how the present invention realizes.For certain miscellaneous Grass, these embodiments show especially significant validity.
A, embodiment
1) missible oil
1.1) active components A, when active constituent B is fenoxapropPethyl.
Formula composition are as follows:+5% calcium dodecyl benzene sulfonate of+5% dimethyl sulfoxide of 6%A+6% fenoxapropPethyl+ 10% phenethyl phenol polyethenoxy ether+100# aromatic solvent naphtha is supplied.
1.2) active components A, when active constituent B is clodinafop-propargyl.
Formula composition are as follows:+10% castor oil of+5% calcium dodecyl benzene sulfonate of+10% isopropanol of 3%A+2% clodinafop-propargyl is poly- Ethylene oxide ether+150# aromatic solvent naphtha is supplied.
The process equipment of above-mentioned missible oil: vacuum pump, batching kettle, storage tank.
The process of above-mentioned missible oil: all materials are put into batching kettle, stirring and dissolving to fully transparent, chemical examination qualification Afterwards, it is filling to be transferred to storage tank.
2) microemulsion
2.1) compound is A, and active constituent B is pinoxaden.
Formula composition are as follows:+4% isooctanol+10% of+10% isopropanol of+10% cyclohexanone of 6%A+3% pinoxaden is along fourth + 5% phenethyl phenol polyethenoxy ether formaldehyde resin condensation product of+10% phenethyl phenol polyethenoxy ether of alkene di-sec-octyl sodium sulfonate+ Water is supplied.
Above-mentioned microemulsion process equipment: vacuum pump, batching kettle, storage tank.
Above-mentioned microemulsion process: raw medicine and solvent are put into batching kettle, stirring and dissolving to fully transparent, Zhi Houjia Enter emulsifier, stir evenly, finally plus water, stirs fully transparent to solution, after chemical examination is qualified, it is filling to be transferred to storage tank.
3) aqueous emulsion
3.1) compound is A, and active constituent B is fluorine pyrrole acyl grass amine.
Formula composition are as follows:+3% phenethyl phenol of+10% cyclohexanone+10%150# solvent naphtha of 3%A+3% fluorine pyrrole acyl grass amine is poly- + 3% ethylene glycol of+3% castor oil polyoxyethylene ether of ethylene oxide ether phosphate+2% phenethyl phenol polyethenoxy ether of triethanolamine salt+ Water is supplied.
Above-mentioned aqueous emulsion process equipment: vacuum pump, batching kettle, storage tank, cutting kettle.
Above-mentioned aqueous emulsion process: raw medicine and solvent are put into batching kettle, stirring and dissolving to fully transparent, Zhi Houjia Enter emulsifier, be stirred for oily phase, ethylene glycol, defoaming agent and water are pumped into cutting kettle later, finally under shearing condition, It is mutually slowly pumped into oily in cutting kettle, after whole materials are pumped into, continues to shear 1 hour, after chemical examination is qualified, be transferred to storage tank filling Dress.
4) suspending agent
4.1) active components A, when active constituent B is diflufenican.
Formula composition are as follows:+0.2% xanthan of+2% pull open powder of 12%A+20% diflufenican+5%EO-PO block polyether + 5% glycerine of glue+water is supplied.
4.2) active components A, when active constituent B is prometryn.
Formula composition are as follows:+5% phenethyl phenol polyethenoxy ether phosphate triethanolamine salt+2% of 6%A+30% prometryn + 0.25%+5% glycerine of xanthan gum of nonylphenol polyoxyethylene ether+water is supplied.
4.3) active components A, when active constituent B is terbutryn.
Formula composition are as follows:+2% fatty alcohol polyoxyethylene ether of+5% naphthalenesulfonate dispersing agent of 6%A+15% terbutryn+ 0.3%+5% glycerine of xanthan gum+water is supplied.
Above-mentioned suspending agent process equipment: mixing kettle, colloid mill, sand mill, cutter etc..
Above-mentioned suspending agent process: all materials are put into mixing kettle, and colloid mill is crossed after being stirred, is entered later Sand mill three-level sanding is finally sheared uniformly in cutter, after chemical examination is qualified, it is filling to be transferred to storage tank.
5) oil-suspending agent can be dispersed
5.1) active components A, when active constituent B is isoproturon.
Formula composition are as follows:+6% phenethyl phenol polyoxyethylene phosphonate triethanolamine salt of 3%A+25% isoproturon+ + 8%+1.5% organobentonite of castor oil polyoxyethylene ether of 6% polyoxyethylene carboxylate+methyl oleate is supplied.
5.2) active components A, when active constituent B is metribuzin.
Formula composition are as follows:+7% Nonyl pheno of+6% maleic di-sec-octyl sodium sulfonate of 6%A+3.5% metribuzin + 2.5%+15% soya-bean oil of organobentonite of+8% castor oil polyoxyethylene ether of ether+methyl oleate is supplied.
5.3) active components A, when active constituent B is mesosulfuron.
Formula composition are as follows:+5% aliphatic alcohol polyoxyvinethene phosphate triethanolamine salt of 6%A+0.6% mesosulfuron+ + 25% soya-bean oil of 5%+2.5% organobentonite of+6% castor oil polyoxyethylene ether of sorbitan fatty acid polyoxyethylene ester+oil Sour methyl esters is supplied.
5.4) active components A, when active constituent B is pyroxsulam.
Formula composition are as follows:+5% calcium dodecyl benzene sulfonate of 6%A+0.8% pyroxsulam+5% sorbitan fatty acid + 2.5%+20% soya-bean oil of fume colloidal silica of+3% organobentonite of+6% castor oil polyoxyethylene ether of polyoxyethylene ester+oleic acid Methyl esters is supplied.
5.5) active components A, when active constituent B is flucarbazone.
Formula composition are as follows:+5% rouge of+5% aliphatic alcohol polyoxyvinethene phosphate triethanolamine salt of 6%A+3% flucarbazone + 3%+20% soya-bean oil of organobentonite of+8% castor oil polyoxyethylene ether of fat alcohol polyoxyethylene ether+methyl oleate is supplied.
Above-mentioned dispersible oil-suspending agent process equipment: mixing kettle, colloid mill, sand mill, cutter etc..
Above-mentioned dispersible oil-suspending agent process: all materials are put into mixing kettle, and colloid mill is crossed after being stirred, Enter sand mill three-level sanding later, is finally sheared in cutter uniformly, after chemical examination is qualified, it is filling to be transferred to storage tank.
6) wettable powder
6.1) active components A, when active constituent B is chlortoluron.
Formula composition are as follows: 3%A+50% chlortoluron+10% naphthalenesulfonate dispersing agent+5% precipitation method of+5% pull open powder are white Carbon black+diatomite is supplied.
Above-mentioned wettable powder process equipment: mechanical crusher, airslide disintegrating mill.
Above-mentioned wettable powder process: raw medicine, auxiliary agent, white carbon black, diatomite etc. are put into mechanical crusher, it Airslide disintegrating mill is crossed afterwards, it is spare after sample examination is qualified.
7) water dispersible granules
7.1) active components A, when active constituent B is tralkoxydim.
Formula composition are as follows:+1% disintegrating agent of+5% pull open powder of+10% polycarboxylic acid salt's dispersing agent of 6%A+30% tralkoxydim is poly- Vinyl alcohol+filler diatomite is supplied.
Above-mentioned water dispersible granules process equipment: airslide disintegrating mill, coulter type mixer, basket pelletizer, drying box, screening Machine etc..
Above-mentioned water dispersible granules process: being uniformly mixed air-flow crushing for above-mentioned material, and water is added to enter to mediate granulation, it After dry, final sizing obtains finished product.
B, pharmacodynamic test
1) experimental condition
1.1) for trying target
(Alopecurus japonicus), Wang careless (Beckmannia syzigachne) picks up from Shandong to Alopecurus Province Huangdao District proving ground wheat paddock.
Above-mentioned weeds are placed in enamel tray using pot-culture method culture with 180 х 140mm plastic nutrition bowls, built-in from agriculture The topsoil (at 4/5) for backing through and air-drying sieving is adopted in field, and soil moisture initial stage controls 20%, and it is uniform to select full seed Weed seed is impregnated 6 hours, the vernalization in 28 DEG C of biochemical cultivation cases (dark), the ruderal species that will have just showed money or valuables one carries unintentionally with 25 DEG C of warm water Son is uniformly placed in soil surface, then earthing 0.7cm.Chemicals treatment is placed on culture in controllable heliogreenhouse, is periodically warding off A certain amount of water is added in porcelain dish, keeps ground moistening.
1.2) condition of culture
It is carried out in controllable heliogreenhouse, 18~30 DEG C of temperature, natural lighting, relative humidity 57%~72%.
Soil types is loam, the content of organic matter 1.63%, pH=7.1, alkali-hydrolyzable nitrogen 84.3mg/kg, rapid available phosphorus 38.5mg/kg, available potassium 82.1mg/kg.
1.3) instrument and equipment
3WP-2000 type walking spray tower, Nanjing Agricultural Machinery Inst., Ministry of Agriculture.GA110 type a ten thousandth electronics day Flat (Germany)；ZDR2000 intelligent data recorder (Hangzhou Ze great Instrument Ltd.)；SPX type Intelligent biochemistry incubator (Ningbo Jiangnan instrument plant).
2) experimental design
2.1) reagent
2.1.1) test medicine
Required active constituent B is commercially available raw medicine, and active components A is 1- (the chloro- 3- of 2- (3- cyclopropyl -5- hydroxyl -1- first Base -1H- pyrazoles -4- carbonyl) -6- trifluoromethyl) piperidines -2- ketone, the compound producing method referring to CN2015107506771, i.e., the following steps are included:
(1) using such as general formula II compound represented and excessive compound R1R2NH is reacted, preparation such as general formula III Compound represented；
(2) it will react such as general formula III compound represented with compound X-A, the chemical combination as shown in general formula I is made Object；
Wherein, A represents halogen, mesyl or p-toluenesulfonyl, R1R2N=R3=R4=Me, X=H, reaction equation are as follows:
The step (1) and (2) carry out in non-protonic solvent, under the action of alkali；Reaction temperature is -30 DEG C - 180℃。
HNMR data are as follows: [DMSO-d6, 500MHz] δ 7.68 (d, J=7.5Hz, 1H), 7.46 (s, 1H), 3.65 (s, 3H),3.39-3.28(m,2H),2.92-2.86(m,1H),2.46-2.35(m,2H),1.68-0.61(m,8H).
Raw medicine is all made of acetone as solvent, is diluted with 0.1% emulsifier T-80 aqueous solution of content, current existing dilution.
2.2) test process
2.2.1) dosage setting
Determining active components A and when active constituent B each group distribution ratio or content, should from the action characters of two kinds of medicaments and Its virulence etc. is measured, it is also contemplated that the main of the formula uses purpose.This research is on the basis of prerun early period, if active constituent A, active constituent B is applied alone and mixes dosage and is shown in Table lattice respectively, designs 15 groups altogether.To be free of medicament, contain same solvent and emulsifier Water as blank control.
2.2.2) test repetition
Every processing is repeated 4 times, 3 basins of each every processing, and every basin sows weed seed 20, totally 60 plants of every processing.
2.3) processing mode
2.3.1 time and number) are handled
It tests and shares medicine 1 time.To 1 heart stage of 2 leaf of weeds, thinning keeps 15 plants of weeds in every basin, and every processing retains 45 plants, It then proceedes to cultivate to Alopecurus, Wang careless 1 heart stage of 3 leaf and be handled.
2.3.2 instrument and administrated method) are used
Cultured test material is uniformly placed in area 0.5m2Platform on, with 3WP-2000 type walking spray tower stem Foliar spray mist, spouting liquid is based on 30 kilograms/hectare.Atomisation pressure 0.3MPa.After whole liquid medicine jets are complete, air valve is closed, after 30 seconds, Spraying pyller is opened, nutritive cube is taken out.Then air valve is opened, clear water 50ml is sprayed, cleans sparge pipe.
3) test method
Using pot-culture method.Weeds culture is shown in 2.1, carries out referring to " farm-chemical indoor determination test rule herbicide ".With Prescription method is shown in 3.3.2, using cauline leaf process method.
4) data survey and statistical analysis
4.1) investigation method
Using absolute number investigation method, the survival whole strain seedling of weeds is cut off along soil surface with blade, is weighed with assay balance Weeds fresh weight.It is based on zero by fresh weight for dead weeds.
4.2) control time and number
It investigates within 20 days after processing, investigates 1 time altogether.
4.3) data statistic analysis
With Gowing method calculate it is each processing hybrid combining theoretical fresh weight inhibition rate (E0=X+Y-X*Y/100), then with Actual measurement inhibiting rate (E) compares, and the mixed synergy type to weeds of both evaluations is made when E-E0 value is greater than 10% for synergy With, be antagonism less than -10%, be addition between -10%~10%.And it is special according to practical preventive effect and herbicide The factors such as the balance of point, formula determine optimum proportioning.
The fresh weight inhibition rate that X is active components A dosage in formula when being P；The fresh weight that Y is active constituent B dosage when being Q inhibits Rate.
Statistical result see the table below.
1 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with isoproturon
2 active components A of the table practical preventive effect and synergy effect (Gowing to weeds mixed with diflufenican Method)
3 active components A of the table practical preventive effect and synergy effect (Gowing to weeds mixed with fluorine pyrrole acyl grass amine Method)
4 active components A of the table practical preventive effect and synergy effect (Gowing to weeds mixed with fenoxapropPethyl Method)
5 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with clodinafop-propargyl
6 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with pinoxaden
7 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with tralkoxydim
8 active components A of the table practical preventive effect and synergy effect (Gowing to weeds mixed with mesosulfuron Method)
9 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with flucarbazone
10 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with pyroxsulam
11 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with metribuzin
12 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with prometryn
13 active components A of the table practical preventive effect and synergy effect (Gowing method) to weeds mixed with terbutryn
The practical preventive effect and synergy effect (Gowing method) of 14 active components A of table and Chlorotoluron to weeds
1) it is tested using herbicidal composition eliminating weed in wheat field made from embodiment 1.1-7.1.
2014 in Henan Zhumadian, Jiangsu Siyang, Anhui is day long, Shouxian County, Anhui Province, the test of the area of wheat 25,5, Jiangsu Xinghua Point carries out exemplary promote and tests.See Table 1 for details 5 for different demonstration area wheat breeds.
The different demonstration area wheat breed situations of table 15
Demonstration area Wheat breed Type
Zhumadian All wheats 26 The white wheat of hard
Siyang Yangmai No.158 The red wheat of hard
It is long Raise wheat 15 The red wheat of hard
Shou County Raise wheat 13 The red wheat of hard
Xinghua Peaceful wheat 13 The red wheat of hard
Test method: after 3 leaf of wheat, 1 heart, the weeds 3-5 leaf phase, hand sprayer, 15 kilograms/667m of the amount of being watered2, use Cauline leaf is sprayed even spraying, and specific test medicine and dosage are shown in Table 16, and 50 square metres of plot area, every processing is repeated 4 times.Application 45 days investigation preventive effects are shown in Table 16 afterwards, and Safe to wheat situation is shown in Table 17.
16 field demonstration effect situation of table
17 field demonstration Safe to wheat situation of table
Note: weed community type in each demonstration pilot project: Zhumadian: Alopecurus+wild avena sativa+Itanlian rye；Siyang: day This amur foxtail+Wang grass+hard grass；It is long: Alopecurus+Wang grass；Shou County: Alopecurus+Wang grass；Xinghua: Alopecurus+ Wang grass+caput grass.
By a large number of experiments and exploration, it is an unexpected discovery of the invention that 1- (the chloro- 3- of 2- (3- cyclopropyl -5- hydroxyl -1- first Base -1H- pyrazoles -4- carbonyl) -6- trifluoromethyl) piperidines -2- herbicides are mixed with active constituent B, it is used for wheat paddock seedling Rear defence removes gramineae weed, has surprising, unexpected synergistic effect, especially careless, hard to Alopecurus, Wang The gramineae weeds such as grass, Itanlian rye have particularly evident synergistic effect, while can reduce dosage, improve crop safety Property, the pollution to environment is reduced, and rationally compounding reduces agricultural cost, there is good prospect.

Claims (11)

1. a kind of Herbicidal combinations, which is characterized in that active components A and active constituent B including herbicidally effective amount, wherein
Active components A is compound
Active constituent B can be selected from one of following compound or a variety of:
1) ureas: isoproturon, chlortoluron；
2) pyridines: diflufenican, fluorine pyrrole acyl grass amine；
3) aryloxyphenoxypropionate class: fenoxapropPethyl, clodinafop-propargyl, alkynes oxalic acid；
4) cyclohexyl diketone: tralkoxydim；
5) sulfonylurea: mesosulfuron, Sulfosulfuron, procarbazone, flucarbazone；
6) triazines: metribuzin, prometryn, terbutryn；
7) sulfonamides: pyroxsulam；
8) phenylpyrrazolin class: pinoxaden.
2. Herbicidal combinations according to claim 1, which is characterized in that the active constituent B be isoproturon, chlortoluron, Diflufenican, fluorine pyrrole acyl grass amine, fenoxapropPethyl, clodinafop-propargyl, tralkoxydim, mesosulfuron, flucarbazone, metribuzin, One of prometryn, terbutryn, pyroxsulam, pinoxaden are a variety of.
3. Herbicidal combinations according to claim 1 or 2, which is characterized in that the weight ratio of A and B is 1-100:1-100.
4. Herbicidal combinations according to claim 1 or 2, which is characterized in that the weight ratio of A and B is 1-50:1-50.
5. Herbicidal combinations according to claim 1 or 2, which is characterized in that the weight ratio of A and B is 1-20:1-20.
6. Herbicidal combinations according to claim 1 or 2, which is characterized in that the quality percentage of A and B in the Herbicidal combinations Content accounts for the 1-95% of total amount.
7. Herbicidal combinations according to claim 6, which is characterized in that the mass percentage of A and B in the Herbicidal combinations Account for the 10-80% of total amount.
8. Herbicidal combinations according to claim 1 or 2, which is characterized in that the specific preparation of the Herbicidal combinations be missible oil, Aqueous suspension agent, microemulsion, suspoemulsion, aqueous emulsion, dispersible oil-suspending agent, wettable powder or water dispersible granules.
9. Herbicidal combinations according to claim 1 or 2, which is characterized in that further include safener C.
10. Herbicidal combinations according to claim 9, which is characterized in that the safener C be selected from mefenpyrdiethyl, cloquintocetmexyl, Isoxadifen, cyclopropyl-sulfonylamide, naphthalic anhydride, chlorine oxalene peace, R-28725, AD-67, CGA-154281, CGA-43089, It is CGA-43089, Hoe-70542, benoxacor, flurazole, BAS-145138, MON-13900, quinoline, 2,4-D, novel One of Antidote T and gibberellin are a variety of.
11. application of the Herbicidal combinations in prevention and treatment injurious weed as described in claim 1-10 any one.
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Publication number Priority date Publication date Assignee Title
WO1997046530A1 (en) * 1996-06-06 1997-12-11 E.I. Du Pont De Nemours And Company Herbicidal pyridinyl and pyrazolylphenyl ketones
CN103980202A (en) * 2014-05-27 2014-08-13 青岛清原化合物有限公司 4-benzoyl pyrazole compound with herbicidal activity

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO1997046530A1 (en) * 1996-06-06 1997-12-11 E.I. Du Pont De Nemours And Company Herbicidal pyridinyl and pyrazolylphenyl ketones
CN103980202A (en) * 2014-05-27 2014-08-13 青岛清原化合物有限公司 4-benzoyl pyrazole compound with herbicidal activity

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