CN106376561A - Microcapsule type pesticide composition - Google Patents
Microcapsule type pesticide composition Download PDFInfo
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- CN106376561A CN106376561A CN201610640964.1A CN201610640964A CN106376561A CN 106376561 A CN106376561 A CN 106376561A CN 201610640964 A CN201610640964 A CN 201610640964A CN 106376561 A CN106376561 A CN 106376561A
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- Prior art keywords
- agent
- trefanocide
- pendimethalin
- microcapsule
- encapsulated form
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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
- A01N33/00—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds
- A01N33/16—Biocides, pest repellants or attractants, or plant growth regulators containing organic nitrogen compounds containing nitrogen-to-oxygen bonds
- A01N33/18—Nitro compounds
-
- 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
- A01N25/00—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests
- A01N25/26—Biocides, pest repellants or attractants, or plant growth regulators, characterised by their forms, or by their non-active ingredients or by their methods of application, e.g. seed treatment or sequential application; Substances for reducing the noxious effect of the active ingredients to organisms other than pests in coated particulate form
- A01N25/28—Microcapsules or nanocapsules
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- Life Sciences & Earth Sciences (AREA)
- General Health & Medical Sciences (AREA)
- Health & Medical Sciences (AREA)
- Wood Science & Technology (AREA)
- Pest Control & Pesticides (AREA)
- Plant Pathology (AREA)
- Engineering & Computer Science (AREA)
- Dentistry (AREA)
- Agronomy & Crop Science (AREA)
- Zoology (AREA)
- Environmental Sciences (AREA)
- Toxicology (AREA)
- Agricultural Chemicals And Associated Chemicals (AREA)
Abstract
The invention discloses a microcapsule type pesticide composition. The microcapsule of the microcapsule type pesticide composition comprises an active component A and an active component B, wherein A is trifuralin, B is pendimetalin, and a weight ratio of A to B is (1-45): (55-1); the wall of the microcapsule at least comprises one active component trifuralin; and the mass content of the active components of the e pesticide composition is 2 to 60%, while the mass content of auxiliary agents is 40 to 98%. Pharmacodynamic test results show that the composition can overcome the problems of degradation under action of light, low drug effect utilization rate and the like of conventional dosage forms of trifuralin; manual or mechanical turning and covering of soil are not needed after spraying of the composition, which enables labor cost to be reduced; and the action period of drug effect is prolonged. The composition has substantial synergistic effect, a broadened weed-control spectrum and improved safety to crops.
Description
Technical field
The invention belongs to agriculture plant protection field, more particularly to a kind of Herbicidal combinations with improvement performance.
Background technology
Trefanocide (trifluralin) is dinitroaniline herbicide before selective bud.Easily wave because trefanocide has
Send out, easy photodissociation, water-soluble minimum, be difficult to move in soil layer, the features such as the lasting period is long, therefore trefanocide is usually used in before seedling soil
Process, it is mainly absorbed with plumular axis by the plumule of weeds and works, invalid to weeds of being unearthed, but to grass family and portion
Divide the broad leaved weed of small-sized seed also effective.Trefanocide is mainly used in preventing and kill off barnyard grass, lady's-grass, eleusine indica, johnson grass Chinese sorghum, a thousand pieces of gold
The annual standing grain such as son, eragrostis cilianensisLink, annual bluegrass, bromegrass, hard grass, caput grass, amaranth, lamb's-quarters, purslane, chickweed, knotweed, Armstrong, puncture multitude
Undergraduate course and part broad leaved weed.This product is substantially carried out before seedling soil treatment, mixes soil immediately after dispenser, in order to avoid medicament volatilization impact
Herbicidal effect.
A kind of outstanding dry crop selective herbicide of pendimethalin (Pendimethalin), can be widely applied to
The field weeding of the various crop such as corn and soybean, peanut, cotton, direct-seeding dry rice, potato, tobacco, vegetables.Pendimethalin is to select
Property bud before, after bud upland field soil process herbicide.The young shoot that weeds pass through sprouting absorbs medicament, enters the medicine in plant body
Agent and tubulin binding, the mitosis of suppression plant cell, thus cause weeds dead.
Because trefanocide is volatile, photodissociation, therefore after dispenser, manually or mechanically must mix soil immediately, this just have impact on fluorine pleasure
The drug effect of spirit, increased the use cost of trefanocide, reduces the market competition status of trefanocide.Simultaneously because chronic administration list
The trefanocide of one activity, leads to the resistance long-term accumulated of trefanocide serious, drug effect reduction.
Content of the invention
The purpose of the present invention is to see that light decomposes when effectively solving trefanocide is applied, and leads to the low problem of drug effect utilization rate, this
Invention need not manually or mechanically be turned over and be taken off blinding, reduce labor cost, simultaneously by compounding trefanocide with pendimethalin, solve
The resistance problem that long-term single administration trefanocide single dose causes, delays the resistance of trefanocide to produce, and the physics and chemistry improving trefanocide is steady
Qualitative, improve utilization rate of active components, extend the drug effect lasting period, improve to crop safety.And between two kinds of active components no
Cross resistance.
The purpose of the present invention can be reached by following measures：
The invention provides a kind of Herbicidal combinations of encapsulated form, said composition comprises effective constituents A and B, activearm
A is divided to be trefanocide, active component B is pendimethalin.
In said herbicidal composition, weight between component A and component B two component is than for 1～45：55～1, preferably 1
～40：50～1, for improving prevention effect further, the weight ratio of component A and component B can further preferred 1～30：45～1.
A kind of active ingredient of trefanocide is at least contained, active ingredient quality in this composition pesticide in the cyst wall of encapsulated form
Content accounts for 2～70%, and remaining is auxiliary agent.The mass content of auxiliary agent accounts for 98%～30%.
Encapsulated form in the present invention is using macromolecular material as cyst wall or cyst membrane, by chemistry, physics or physico
The method learned, wraps up after the pesticide activity component solvent dissolving as capsule-core, forms one kind and have semipermeability capsule
The microencapsulation (abbreviation micro-capsule) of film.In the cyst wall of encapsulated form of the present invention, (i.e. capsule-core) necessarily comprises active ingredient trefanocide,
Different according to subject, and the difference of the careless phase of effect, capsule-core can also comprise active ingredient pendimethalin.According to above-mentioned think of
Road, the suitable encapsulated form of the present invention mainly includes：Microcapsule suspending agent, micro-capsule suspension emulsion, microcapsulated granule, microcapsule suspension-suspension
Agent, microcapsule suspension-aqueous emulsion and microcapsule suspension-suspension emulsion.
In the microcapsule suspending agent of the suitable present invention, micro-capsule suspension emulsion or microcapsulated granule, the capsule-core of encapsulated form comprises effectively
Composition trefanocide and the mixture of pendimethalin；Or first prepare the bag containing active ingredient trefanocide or pendimethalin respectively
Capsule, then two kinds of packings are formed microcapsule suspending agent, micro-capsule suspension emulsion or microcapsulated granule in the ratio mixing of two kinds of active ingredients
Micro-capsule part；In the microcapsule suspension-suspendinagent agent of the suitable present invention, microcapsule suspension-aqueous emulsion or microcapsule suspension-suspension emulsion,
The micro-capsule containing active ingredient trefanocide can first be prepared, by active ingredient pendimethalin be prepared into suspension (or claim suspend
Agent), emulsion (or claim water float agent) or suspended emulsion (or claiming suspension emulsion).
The microcapsule suspending agent of the suitable present invention, micro-capsule suspension emulsion or microcapsulated granule formulation it is characterised in that cyst wall in (i.e. capsule
Core) comprise the mixture according to a certain percentage by active ingredient trefanocide and pendimethalin, both will be mixed and made into miniature glue
Capsule.Microencapsulation is stably disperseed using certain concentration, is suspended in the formation microcapsule suspending agent as in the water of continuous phase.Pass through
Spray-drying process or extruding granulation drying, can obtain pesticide micro-capsule granules.Micro-capsule suspension emulsion can select with lower section
Prepared by formula：First prepare the microcapsule suspending agent containing trefanocide and pendimethalin according to the method described above, treat standby.By emulsifying agent, thickening
The auxiliary agents such as agent, defoamer are added to the water and are evenly stirred until and are completely dissolved, and add the microcapsule suspending agent preparing, are mixed with high speed shear
Clutch high speed shear mixes and obtains final product micro-capsule suspension emulsion.
Or, first prepare the packing containing active ingredient trefanocide or pendimethalin respectively, then two kinds of packings (prepared
The good microencapsulation containing trefanocide and the microencapsulation containing pendimethalin) mix composition in the ratio of two kinds of active ingredients
The micro-capsule part of microcapsule suspending agent, micro-capsule suspension emulsion or microcapsulated granule；Mixture is stably disperseed with certain concentration,
It is suspended in as formation microcapsule suspending agent in the water of continuous phase.Also can be obtained by said method with the microcapsule suspending agent that this is obtained
Pesticide micro-capsule granules and micro-capsule suspension emulsion.
Specific preparation technology can select following methods：
1st, prepare microcapsule suspending agent first, comprise the following steps：Trefanocide and pendimethalin active compound are proportionally mixed
Heating melting adds appropriate oil phase Encapsulating materials to be uniformly mixing to obtain oil phase；It is previously added wetting agent in water, dispersant stirs
Mix uniformly, be subsequently adding pre-configured oil phase, high speed homogenizing formation stabilized oil-in-water emulsion；Reduce rotating speed, add cyst wall
Material, controlling reaction temperature, in 18 DEG C～85 DEG C, keeps 1.5 hours～24 hours, makes cyst material solidify encystation.Treat encystation
After material is fully cured encystation, adds PH acid-base modifier, adjust to required pH range, add appropriate dispersant, disappear
The adjuvants such as infusion, stir and make microcapsule suspending agent；
2nd, the microcapsule suspending agent preparing is obtained micro-capsule granules by drying-granulating.Specifically include following steps：First
First previously prepared microcapsule suspending agent is stirred together with dispersant, wetting agent, disintegrant and filling carrier etc., adjust it
Concentration and viscosity, obtain the slurry sprayed；Then slurry is become small drop through nozzle atomization, sprays in automiser spray,
Hot-air enters drier with drop ejection cocurrent or countercurrent；Clean hot-air is mixed simultaneously with material in Granulation Equipments with slip
Moisture in evaporation slip, forms micro-capsule granules.
Described drying-granulating mainly obtains micro-capsule by extruder grain method or two kinds of granulating and drying modes of spray drying process
Granule, wherein：Extruder grain method refers to by carrier filler, microcapsule suspending agent be adsorbed, and is subsequently adding wetting agent, divides
The adjuvants such as powder, disintegrant, then extruder grain, obtain microcapsulated granule finally by fluidized drying；Spray drying process refers to directly
Connect using microcapsule suspending agent slip Direct spraying drying and granulating, finally give micro-capsule granules.
Active ingredient trefanocide can be prepared into micro-capsule and hang by the microcapsule suspension-suspendinagent agent of the present invention according to the method described above
Floating agent, active ingredient pendimethalin is prepared into suspending agent, and both are proportionally prepared by mixing into microcapsule suspension-suspendinagent agent.Tool
The preparation method of body can be：In reaction vessel, trefanocide is dissolved in cosolvent, is subsequently adding solvent, cyst material etc. and helps
After high-speed stirred is uniform after agent, add initiator, agitated, progressively it is warming up to, containing trefanocide microcapsule suspension is obtained.By diformazan
Penta spirit is sufficiently mixed, disperses with auxiliary agent and water, then sand milling, obtains pendimethalin suspension (or claiming suspending agent), and trefanocide is micro-
Capsule suspension is sufficiently mixed, stirs, disperses with pendimethalin suspension, obtains final product the microcapsule suspension of trefanocide pendimethalin-outstanding
Floating agent.
Active ingredient trefanocide can be prepared into microcapsule suspending agent, by active ingredient by the microcapsule suspension-aqueous emulsion of the present invention
Pendimethalin is prepared into aqueous emulsion (or referred to as aqueous emulsion), and both are proportionally prepared by mixing into microcapsule suspension-aqueous emulsion.Specifically
Technique can adopt following methods：First trefanocide is heated to melting and is used for making capsule-core, add cyst material to stir,
Then online-emulsification is carried out using emulsion dispersion equipment, obtain microcapsule particle；Microcapsule particle after emulsification and curing agent occur anti-
Should, and add dispersant to form stable trefanocide microcapsule suspending agent (mother liquor)；Sexual element is added in microcapsule suspension mother liquor
The auxiliary agents such as pendimethalin, emulsifying agent, antifreeze and water, pass through high-speed emulsifying machine after mixing, obtain microcapsule suspension-water and milk
Agent.
Active ingredient trefanocide can be prepared into microcapsule suspending agent by the microcapsule suspension-suspension emulsion of the suitable present invention, will be effectively
Composition pendimethalin is prepared into suspension emulsion (or referred to as suspended emulsion), and both are proportionally prepared by mixing into microcapsule suspension and hang breast
Agent.Concrete technology can adopt following methods：(1) trefanocide is dissolved in cosolvent, is subsequently adding auxiliary agent, solvent and cyst material
After high-speed stirred is uniform, add initiator, agitated, progressively it is warming up to, containing trefanocide microcapsule suspending agent is obtained, taking-up is treated standby
With.(2) water is mixed with wetting dispersing agent, antigraining agent, defoamer, after input pendimethalin is uniformly dispersed, by sand
Grinding machine carries out serialization sand milling, obtains the suspending agent of pendimethalin；(3) emulsifying agent is dissolved in sticker, after mixing
Obtain oil phase, emulsifying agent and water are mixed and made into aqueous phase, the oil phase having configured are poured into aqueous phase and opens high speed homogenizing, formed steady
Fixed O/W emulsion；(4) emulsion adding step (2) to obtain in the pendimethalin suspension preparing, mixes, obtains
Pendimethalin suspension emulsion.(5) trefanocide microcapsule suspending agent is mixed with pendimethalin suspension emulsion and obtain final product containing trefanocide two
Microcapsule suspension-the suspension emulsion of first penta spirit.
Auxiliary agent in encapsulated form of the present invention includes into one or more of wafer and following auxiliary agent：Emulsifying agent, profit
Humectant, dispersant, initiator, filler, stabilizer, curing agent, solvent and auxiliary addition agent, but the auxiliary agent in the present invention does not limit to
In above-mentioned various, also can add other kinds of auxiliary agent when necessary, such as adhesive, viscosity modifier etc..
The material of the cyst wall part of the encapsulated form of the suitable present invention, wafer can be selected from carbohydrate, egg
White matter class or lipid become wafer；One-tenth wafer can be directly using it is also possible to add encystation monomer with end form in preparation process
Encystation wall part.Suitable carbohydrate become wafer can selected from converted starch, maltodextrin, corn syrup, cyclodextrin,
Sucrose, lactose, aspergillus polysaccharide, cellulose, colloid or glucan；Suitably protein-based one-tenth wafer can be selected from gelatin, soybean
Albumen, lactalbumin, network protein acid sodium, glutelin, peptide, gliadin, hemoglobin or egg white powder etc.；Suitable fat
Class becomes wafer can be selected from paraffin, beeswax, hard triglycerides, monoglyceride, diglyceride, oil, fat, carbamide resin, hydrogenation
Oil, lecithin, polyurethane, Lauxite, polyesteramide, Arabic gum, melamine resin, aliphatic polyamide resin, poly- acetic acid
One of vinyls or polystyrene resin.
The suitable preferred hydrochloric acid of initiator, glacial acetic acid, fatty glyceride, lactolactone and amino acid ammonium chloride, second two
Amine, 1- octyne -3- alcohol, triethylamine, glyceride lactate, or triethanolamine and acid regulator known in those skilled in the art
Or a kind of or arbitrarily several combination of alkaline conditioner.
Suitable solvent preferred methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil, methyl esters coconut oil, rosin-based plant
One of oil ＆ fat acid esters, or one of toluene, acetone, isopropanol, chloroform, ethanol, methyl alcohol, hexamethylene or two kinds
Any of the above mixes.Most preferably methyl esters soybean oil, methyl esters palm oil, turpentine-based vegetable oil.
Suitable curing agent preferably following component one or more：Double bond containing alcohol ether sulfosuccinates
Sodium salt, allyl alcohol ether sulfate, allyl ether hydroxypropanesulfonic acid sodium, sodium vinyl sulfonate, alkyl phenol allyl polyether sulphur
Hydrochlorate acrylamido sodium isopropyl xanthate, 2- allyl ether 3- base propane -1- sodium sulfonate and allyl polyether sulfate.
The suitable preferred epoxidized soybean oil of stabilizer, 2,6- toluene di-tert-butyl phenol (BHT), butylated hydroxy anisole
(BHA), one of triphenyl phosphite and potassium dihydrogen phosphate.
Suitable dispersant optimization aromatic sulfonate, acrylic acid and acrylic ester copolymers, formaldehyde condensate sulfonate,
Copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt, styrene alkyl polyoxyethylene ether phosphate, naphthalene sulfonate formaldehyde condensation
Thing, triphenyl vinyl phenol polyethenoxy ether class and derivative eater, fatty alcohol polyethenoxy ether class, APES
Class, macromolecule EO-PO block copolymer, lignosulfonates, alkylphenol-polyethenoxy formaldehyde condensation products sulfate, alkyl phenol gather
Oxygen vinethene formaldehyde condensation products sulfate phosphates, styrene phenol formaldehyde resin polyoxyethylene ether phosphate salt, styryl
Phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates, macromolecule dredge dress copolymer, the polymerization of carboxylic acid salt of type
Being applied in combination of one or more of class.
Suitable emulsifying agent preferred anhydrous sorbitol laurate, polyoxyethylene laurel ether, AEO, poly-
Oxygen ethene monopalmitate and one kind of Emulsifier EL-60.
Suitable filler be selected from modified water-soluble starch, cellulose ether and its derivative, aluminium-magnesium silicate, kaolin, diatomite,
One of attapulgite, glucose, precipitated calcium carbonate, white carbon, inorganic salts.
Suitable wetting agent preferably sodium dodecyl sulfate, Nonyl pheno, alkylphenol-polyethenoxy formaldehyde condensation
Thing sulfate, APES formaldehyde condensation products sulfat phosphate, styrene phenol formaldehyde resin APEO
Phosphate ester salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates, dialkyl succinylsuccinate ester sulfonic acid
One of salt, this disk SPAN, soil temperature TWEEN or two or more being applied in combination.
Suitable adjuvant is selected from binding agent, disintegrant, PH conditioning agent, sterilization antiseptic, defoamer, antifreeze, thickening
The combination of one or more of agent；Wherein：Described binding agent is selected polyvinyl alcohol, gelatin, Arabic gum, xanthans, is gathered
One kind of PAA, sodium alginate, starch, cellulose and its derivates, preferred cellulose and its cellulose derivative；Disintegration
Agent is selected from aluminium-magnesium silicate, polyethylene glycol PEG, modified starch, inorganic salts, White Carbon black, one kind of silica gel；Described PH soda acid is adjusted
Section agent is one of glacial acetic acid, hydrochloric acid, ammoniacal liquor, monoethanolamine, triethanolamine；Described sterilization antiseptic is：Potassium sorbate, benzene
One of sodium formate, formaldehyde, isothiazolinone；Described defoamer：Natural oil, polyethers defoamer, higher alcohols, organic
One kind of silicon defoaming agent.Described antifreeze is selected from propane diols or ethylene glycol；Described thickener be selected from xanthans, carragheen, pectin,
Agar, algin or sodium carboxymethylcellulose.
In the composition of the present invention, two kinds of active ingredients show as synergistic effect, and the activity of said composition is than using individualized
The expected summation of activity of compound, and the individually activity of single compound is more notable.Synergistic effect shows as allowing amount of application
Reduce, broader weeding controls spectrum, instant effect, more longlasting prevention effect, pass through only once or minority is applied more preferably several times
Control weeds and broaden the possible administration interval time.These characteristics are to prevent and kill off in control weeds practice process especially
Need.Therefore the composition pesticide of the encapsulated form of the present invention can be applicable to agriculture field preventing and treating crop weeds aspect.
The other features showing of the encapsulated form Herbicidal combinations of the present invention are mainly shown as：1st, pass through encapsulated form
Solve to see that light decomposes when trifluralin ec is applied, the low problem of utilization rate of active components；2nd, trifluralin ec needs machine when applying
To reduce trefanocide, tool or manually turn over and take off earthing, is shown in that light decomposes, the encapsulated form of the present invention need not manually be digged after applying, permissible
Reduce labor cost；3rd, because two single dose chemical constitutions of this composition are widely different, the mechanism of action is entirely different, both
Between synergistic effect substantially, there is not cross resistance, two single doses can be delayed to be used alone produced resistance problem；4th, originally
Invention, by trefanocide is become encapsulated form with pendimethalin Combined machining, can extend the lasting period, when improving trefanocide administration
Stability and crop security, improve utilization rate of active components.
Specific embodiment
In order that the objects, technical solutions and advantages of the present invention become more apparent, with reference to embodiments, to the present invention
It is further elaborated.It should be appreciated that specific embodiment described herein, only in order to explain the present invention, is not used to limit
Determine the present invention, all any modification, equivalent and improvement made within the spirit and principles in the present invention etc., should be included in
Within protection scope of the present invention.
In all formulas of following examples, percentage is all weight percentage.The processing work of the various preparation of the present composition
Skill is prior art, can be varied from according to different situations.
First, formulation preparation embodiment
(1) processing of microcapsule suspending agent
Embodiment 1 55% trefanocide pendimethalin microcapsule suspending agent (active components A：Active component B=45:10)
By active ingredient trefanocide 45%, pendimethalin 10%, it is added in 12% solvent rosinweed oil and stirs,
After add stabilizer triphenyl phosphite 1.8%, emulsifier polyoxyethylene castor oil 2%, initiator glyceride lactate
1.5%, add encystation monomer toluene di-isocyanate(TDI) 10% to be uniformly mixing to obtain oil phase；By dispersant acrylic acid-acrylic ester
Copolymer 2.5% is added to the water with antifreeze propane diols 2%, preservative sodium benzoate 0.3%, thickener xanthans 1.8%
(water complements to 100%) is uniformly mixing to obtain aqueous phase；Oil, water are preheated to 45 DEG C, then pour oil phase into aqueous phase and open height
Speed emulsification, when stable emulsion, keeping temperature 4 hours, obtains, using interfacial polymerization, 50% fluorine that carbamide resin is capsule material
Happy spirit pendimethalin microcapsule suspending agent (active components A：Active component B=45:10).
Embodiment 2 55% trefanocide pendimethalin microcapsule suspending agent (active components A：Active component B=10:45)
By active ingredient trefanocide 10%, pendimethalin 45%, add in solvent methyl esters soybean oil 13% and stir, after
Add stabilizer epoxidized soybean oil 2%, emulsifying agent AEO 1.5%, initiator 1- octyne -3- alcohol 0.8%,
Encystation monomer toluene di-isocyanate(TDI) 11% is added to be uniformly mixing to obtain oil phase；By dispersant polymerization of carboxylic acid sodium salt 2% with anti-
Freeze agent ethylene glycol 2%, preservative KF88 1.8%, thickener xanthans 0.8% are added to the water (water complements to 100%) stirring
Uniformly obtain aqueous phase.Oil, water are preheated to 40 DEG C, then pour oil phase into aqueous phase and open emulsification at a high speed, obtain stable breast
Liquid, keeping temperature 6 hours, microcapsule suspending agent 55% trefanocide two that capsule material for carbamide resin is is obtained using interfacial polymerization
Clever microcapsule suspending agent (the active components A of first penta：Active component B=10:45).
Embodiment 3 31% trefanocide pendimethalin microcapsule suspending agent (active components A：Active component B=30:1)
By active ingredient trefanocide 30%, pendimethalin 1%, it is added in solvent 15% rosinweed oil and stirs,
After add emulsifier polyoxyethylene bay ether 6%, initiator fatty glyceride 4% is uniformly mixing to obtain oil phase；Antifreeze
Glycerine 4.5%, stabilizer potassium dihydrogen phosphate 1%, encystation performed polymer formaldehyde-urea performed polymer 14% are added to the water, and (water is mended
Enough to 100g) it is uniformly mixing to obtain aqueous phase；Oil, water are preheated to 60 DEG C, then pour oil phase into aqueous phase and open emulsification at a high speed,
When stable emulsion, add watery hydrochloric acid to adjust pH=2.5 in batches and polycondensation reaction, keeping temperature 4 hours occur, then will disperse
Agent sodium lignin sulfonate 3%, thickener carragheen 0.2%, preservative sodium benzoate 0.8% addition stir, and change example and adopt
Obtain the 3 1% trefanocide pendimethalin microcapsule suspending agent (active components A that Lauxite is capsule material with situ aggregation method：Live
Property composition B=30:1).
Embodiment 4.31% trefanocide pendimethalin microcapsule suspending agent (active components A：Active component B=1:30)
By active ingredient trefanocide 1%, pendimethalin 30%, it is added in solvent 21% methyl esters coconut oil and stirs,
After add stabilizer BHT2%, emulsifier polyoxyethylene monopalmitate 2%, initiator amino acid/11 .5% stirs
To oil phase；By dispersant lignosulfonates 5% and antifreeze glycerine 4%, preservative KF88 3%, the poly- acetic acid of Encapsulating materials
Vac emulsion 3%, thickener xanthans 1% be added to the water (water complements to 100g) be uniformly mixing to obtain aqueous phase；Will be pre- to oil, water
Heat, to 60 DEG C, is then poured oil phase into aqueous phase and is opened emulsification at a high speed, when stable emulsion, keeping temperature 4 hours, using outstanding
Floating polymerization obtains the 31% trefanocide pendimethalin microcapsule suspending agent (active components A that polyvinyl acetate resin is capsule material：Live
Property composition B=1:30).
(2) processing of micro-capsule suspension emulsion
Preparation method：(1) trefanocide is dissolved in cosolvent, is subsequently adding auxiliary agent, solvent and cyst material high-speed stirred equal
After even, add initiator, agitated, progressively it is warming up to, containing trefanocide microcapsule suspending agent is obtained, taking-up is treated standby.(2) by water with
Wetting dispersing agent, antigraining agent, defoamer mix, and after input pendimethalin is uniformly dispersed, are carried out continuously by sand mill
Change sand milling, obtain the suspending agent of pendimethalin；(3) emulsifying agent is dissolved in sticker, after mixing, obtains oil phase, by breast
Agent and water are mixed and made into aqueous phase, the oil phase having configured is poured into aqueous phase and opens high speed homogenizing, form stable O/W emulsion；
(4) emulsion adding step (2) to obtain in the pendimethalin suspension preparing, mixes, and obtains pendimethalin and hangs breast
Agent.(5) trefanocide microcapsule suspending agent is mixed, with pendimethalin suspension emulsion, the micro-capsule obtaining final product containing trefanocide pendimethalin
Suspension-suspension emulsion.
Embodiment 5 35% trefanocide pendimethalin micro-capsule suspension emulsion (active components A：Active component B=30:5)
Formula：Trefanocide 30%, pendimethalin 5%, Tripolyglycerol monostearates 2.3%, the poly- second of epoxidized soybean oil 1%
Alkene ether 1.8%, mineral oil 3.8%, methyl esters soybean oil 13%, emulsifying agent AEO 2%, ethylene glycol 1%, initiation
Agent 1- octyne -3- alcohol 0.8%, preservative KF88 2%, toluene di-isocyanate(TDI) 10%, polymerization of carboxylic acid sodium salt 1%, thickener
Xanthans 1%.
The micro- 35% capsule suspension emulsion (active components A of embodiment 6 trefanocide pendimethalin：Active component B=5:30)
Formula：Trefanocide 5%, pendimethalin 30%, by Tripolyglycerol monostearates 2%, polyvinylether 2.5%, ore deposit
Thing oil 3.5%, alkyl naphthalene sulfonic acid condensation polymer sodium salt 3.1%, agent polyvinyl alcohol 2.5%, organic silicon defoamer 2.8%, fatty alcohol
APEO 1.2%, xanthans 0.8%, OIT 1.2%.
(3) processing of microcapsulated granule
Embodiment 7 trefanocide pendimethalin 10% microcapsulated granule (active components A：Active component B=15:1)
First prepare pendimethalin containing trefanocide 16% microcapsule suspending agent using the processing method of microcapsule suspending agent of the present invention
(15%+1%).By the trefanocide preparing pendimethalin 10% microcapsule suspending agent and filler diatomite 61%, ammonium sulfate
18%th, binding agent hydroxyethyl cellulose 1%, wetting agent Nonyl pheno 4.5%, disintegrant aluminium-magnesium silicate 2%, dispersant
The stirring of acrylic acid and acrylic ester copolymers 3.5% grade is mediated uniformly, by extruder grain, the particle diameter 1mm sending～
2.5mm, dries finally by boiling, screening, obtains outward appearance yellowish-brown, moisture controls 2.5% about, content 5% fluorine is found pleasure in
Clever pendimethalin microcapsulated granule.
Embodiment 8 trefanocide pendimethalin 10% microcapsulated granule (active components A：Active component B=1:15)
First prepare pendimethalin containing trefanocide 10% microcapsule suspending agent using the processing method of microcapsule suspending agent of the present invention
(1%+15%).By the trefanocide preparing pendimethalin 10% microcapsule suspending agent and filler white carbon 55.2%, wetting agent
Dialkyl succinylsuccinate sulfonated ester 3.8%, ammonium sulfate 18%, polyvinyl alcohol 3%, disintegrant polyethylene glycol 3%, dispersant triphen second
The stirring of thiazolinyl phenol polyethenoxy ethers 2% grade is mediated uniformly, by extruder grain, the particle diameter 1mm～2.5mm sending,
Pass through afterwards boiling dry, screening, obtain outward appearance yellowish-brown, moisture controls 2.5% about, content 5% trefanocide diformazan penta
Clever microcapsulated granule.
(3) processing of microcapsule suspension-suspendinagent agent
Embodiment 9 42% trefanocide pendimethalin microcapsule suspension-suspendinagent agent (active components A：Active component B=40:
2)
First, first prepare trefanocide 40% microcapsule suspending agent using the processing method of microcapsule suspending agent of the present invention.Diformazan penta
Clever active compound 2%, wetting agent styryl phenol polyethenoxy polyethenoxy ether 8%, dispersant naphthalenesulfonic acid-formaldehyde condensate 5%,
Organic silicon defoamer 3% is sufficiently mixed, disperses with appropriate water, is passed through sand mill sand milling after being uniformly dispersed, and sand milling is to average grain
Footpath 1-5 micron, then add 40% microcapsule suspending agent of prior preparation, ethylene glycol 3%, 6% gram of glacial acetic acid (pH adjusting agent),
3% gram of OIT (mould inhibitor), thickener xanthans colloidal solution 1.5% and water are sufficiently mixed, and dispersed with stirring is uniformly
For the present invention 42% trefanocide pendimethalin microcapsule suspension-suspendinagent agent.
Embodiment 10 55% trefanocide pendimethalin microcapsule suspension-suspendinagent agent (active components A：Active component B=2:
53)
Formula：Trefanocide 2%, pendimethalin 53%, ethanol 3%, ethylenediamine 2%, triethylamine 1%, naphthalene sulphonate formaldehyde
Condensation product 3%, gelatin 11%, water complements to 100%.
Preparation method：The processing method of the present embodiment is same as Example 9, except for the difference that active ingredient proportioning and auxiliary agent.
First prepare trefanocide 2% microcapsule suspending agent, pendimethalin is prepared into 40% suspending agent, both obtain final product 42% after mixing
Trefanocide pendimethalin microcapsule suspension-suspendinagent agent (active components A：Active component B=2:40).
(4) processing of microcapsule suspension-suspension emulsion
Preparation method：First, first prepare trefanocide microcapsule suspending agent using the processing method of microcapsule suspending agent of the present invention, temporarily
It is set to I.Emulsifying agent, thickener, defoamer are added to the water and are evenly stirred until and are completely dissolved, take out standby, fix tentatively as II.Diformazan
It is evenly stirred until in penta spirit addition solvent and is completely dissolved, take out standby, fix tentatively as III.III is added in II, high speed shear, then plus
Enter I, mix and obtain final product trefanocide pendimethalin microcapsule suspension-suspension emulsion.
Embodiment 11 37% trefanocide pendimethalin microcapsule suspension-suspendinagent agent (active components A：Active component B=35:
2)
Formula：Trefanocide 35%, pendimethalin 2%, Lauxite 21%, sodium lignin sulfonate 3%, detergent alkylate sulphur
Acid 5%, Tripolyglycerol monostearates 1%, polyvinylether 2%, mineral oil 1%, balance of water.
Embodiment 12 37% trefanocide pendimethalin microcapsule suspension-suspendinagent agent (active components A：Active component B=2:
35)
Formula：Trefanocide 35%, pendimethalin 2%, succinate sulfonate 3.8%, ammonium sulfate 18%, polyvinyl alcohol,
DBSA 2%, naphthalenesulfonate formaldehyde condensation compound 3%, balance of water.
(4) processing of microcapsule suspension-aqueous emulsion
Preparation method：First trefanocide is heated to melting dress and is used for making capsule-core, add cyst material to stir, so
Afterwards online-emulsification is carried out using emulsion dispersion equipment, obtain microcapsule particle；Microcapsule particle after emulsification and curing agent react,
And add dispersant to form stable trefanocide microcapsule suspending agent (mother liquor)；Sexual element diformazan is added in microcapsule suspension mother liquor
Auxiliary agent and the water such as penta spirit, emulsifying agent, antifreeze, pass through high-speed emulsifying machine after mixing, obtain trefanocide pendimethalin micro-
Capsule suspension-aqueous emulsion.
Embodiment 13 44% trefanocide pendimethalin microcapsule suspension-aqueous emulsion (active components A：Active component B=40:
2)
Formula：Trefanocide 40%, pendimethalin 4%, polyvinyl alcohol 2%, Emulsifier EL-60 4%, glycerine 2%,
Methyl methacrylate 25%, styrene-succinic anhydride copolymer sodium 1%, anhydrous sorbitol laurate 2%, balance of water.
Embodiment 14 44% trefanocide pendimethalin microcapsule suspension-aqueous emulsion (active components A：Active component B=4:
40)
Formula：Trefanocide 2%, pendimethalin 40%, methyl methacrylate 22%, allyl polyether sulfate 3%, horse
Come acid anhydride copolymer sodium salt 3%, polyoxyethylene monopalmitate 1%, urea 3%, xanthans 2%.
2nd, drug effect checking test
(1) Assays Example 1
1st, trefanocide and pendimethalin compound the toxicity test test to shepherd's purse
Using trefanocide as standard agent, calculate disease index and prevention effect.Prevention effect is converted into niqueMin
Y (), liquid is done height (μ g/ml) and is converted into logarithm value (x), calculates concentration in virulence equation and suppression with least square method
EC50, calculates toxicity index level co-toxicity coefficient (CTC) of medicament according to the abundant method of Sun Yun.Toxicity test the results are shown in Table 1.
Actual measurement toxicity index (ATI)=(standard agent EC50/ reagent agent EC50) * 100
Percentage composition+B medicament toxicity index * the mixture of A in theoretical toxicity index (TTI)=A medicament toxicity index * mixture
The percentage composition of middle B
Co-toxicity coefficient (CTC)=[mixture actual measurement toxicity index (ATI)/mixture theoretical toxicity index (TTI)] * 100
CTC≤80, composition shows as antagonism, 80 ＜ CTC ＜ 120, and composition shows as summation action, CTC >=
120, composition shows as synergistic effect.
Table 1 trefanocide and pendimethalin different ratio compound the toxicity test analysis to shepherd's purse
| Medicament title | EC50(μg/ml) | ATI | TTI | Co-toxicity coefficient (CTC) |
| Trefanocide | 7.25 | / | / | |
| Pendimethalin | 6.11 | 118.658 | / | / |
| Proportioning trefanocide and pendimethalin=30:1 | 5.18 | 139.961 | 100.602 | 139.124 |
| Proportioning trefanocide and pendimethalin=20:1 | 4.67 | 155.246 | 100.889 | 153.878 |
| Proportioning trefanocide and pendimethalin=10:1 | 2.87 | 252.613 | 101.696 | 248.400 |
| Proportioning trefanocide and pendimethalin=1:1 | 2.88 | 251.736 | 109.33 | 230.253 |
| Proportioning trefanocide and pendimethalin=1:10 | 3.27 | 221.713 | 116.964 | 189.556 |
| Proportioning trefanocide and pendimethalin=1:20 | 3.84 | 188.802 | 117.771 | 160.313 |
| Proportioning trefanocide and pendimethalin=1:30 | 4.5 | 161.111 | 118.058 | 136.468 |
Result (table 1) shows, trefanocide and pendimethalin are in proportioning 30:1～1:30, co-toxicity coefficient, all more than 135, is said
Bright trefanocide is compounded with pendimethalin has significant synergistic function to preventing and kill off of Soybean Field shepherd's purse.
2nd, trefanocide and pendimethalin compound the toxicity test test to lady's-grass
Table 2 trefanocide compounds the toxicity test interpretation of result to weeds lady's-grass with pendimethalin
| Medicament title | EC50(μg/ml) | ATI | TTI | Co-toxicity coefficient (CTC) |
| Trefanocide | 6.820 | 100.000 | / | / |
| Pendimethalin | 4.350 | 156.782 | / | / |
| Proportioning trefanocide and pendimethalin=30:1 | 4.250 | 160.471 | 101.832 | 157.584 |
| Proportioning trefanocide and pendimethalin=20:1 | 3.660 | 186.339 | 102.704 | 181.433 |
| Proportioning trefanocide and pendimethalin=10:1 | 2.250 | 303.111 | 105.162 | 288.233 |
| Proportioning trefanocide and pendimethalin=1:1 | 2.430 | 280.658 | 128.391 | 218.597 |
| Proportioning trefanocide and pendimethalin=1:10 | 2.230 | 305.830 | 151.620 | 201.708 |
| Proportioning trefanocide and pendimethalin=1:20 | 2.340 | 291.453 | 154.078 | 189.159 |
| Proportioning trefanocide and pendimethalin=1:30 | 2.900 | 235.172 | 154.950 | 151.773 |
Result (table 2) shows, trefanocide and pendimethalin are in proportioning 30:1～1:30, co-toxicity coefficient, all more than 150, is said
Bright trefanocide is compounded with pendimethalin has significant synergistic function to preventing and kill off of weeds lady's-grass.
(2) field control effectiveness test
1st, the embodiment of the present invention is utilized to verify the encapsulated form field control effect of trefanocide and pendimethalin.
Expected preventive effect (%)=X+Y-XY/100 (wherein, X, Y are single dose preventive effect)
Table 3. trefanocide compounds the field efficiency test result to bog pondweed with pendimethalin
Measurement result (table 3) shows, trefanocide compounds the preventive effect to controlling weeds bog pondweed and short arrowhead with pendimethalin
Significantly improve, illustrate that the two compounding has significant synergistic function to weeds bog pondweed and short arrowhead.After medicine, investigation in 60 days is sent out
Existing, the composition of the encapsulated form of the present invention will be significantly higher than comparison medicament to the preventive effect of bog pondweed, and the holding effect of the present invention is described
Phase is longer.The composition of the present invention, when soil is sprayed, takes off earthing it is not necessary to turn over, greatly for trifluralin ec simultaneously
Save greatly labor cost.
Claims (11)
1. it is characterised in that the active ingredient in said composition comprises A and B, wherein A is a kind of composition pesticide of encapsulated form
Trefanocide, B is pendimethalin, and the weight of A and B ratio is for 1～45：55～1, at least contain trefanocide one in the cyst wall of encapsulated form
Plant active ingredient, in this composition pesticide, active ingredient mass content accounts for 2～70%, remaining is auxiliary agent.
2. the composition pesticide of encapsulated form according to claim 1 is it is characterised in that the weight ratio of effective constituents A and B
For 1～40：50～1；Preferably 1～30：45～1.
3. the composition pesticide of encapsulated form according to claim 1 is it is characterised in that auxiliary agent bag in this encapsulated form
Include into one or more of wafer and following auxiliary agent：Emulsifying agent, wetting agent, dispersant, initiator, filler, stabilizer, solid
Agent, solvent and auxiliary addition agent.
4. the composition pesticide of encapsulated form according to claim 3 is it is characterised in that described one-tenth wafer is selected from carbon aquation
Compound class, protein-based or lipid become wafer；Described carbohydrate becomes wafer to be selected from converted starch, maltodextrin, corn
Syrup, cyclodextrin, sucrose, lactose, aspergillus polysaccharide, cellulose, colloid or glucan；Described protein-based one-tenth wafer is selected from bright
Glue, soybean protein, lactalbumin, network protein acid sodium, glutelin, peptide, gliadin, hemoglobin or egg white powder；Institute
Stating lipid becomes wafer to be selected from paraffin, beeswax, hard triglycerides, monoglyceride, diglyceride, oil, fat, carbamide resin, hydrogenation
Oil, lecithin, polyurethane, Lauxite, polyesteramide, Arabic gum, melamine resin, aliphatic polyamide resin, poly- acetic acid
One of vinyls or polystyrene resin.
5. the composition pesticide of encapsulated form according to claim 3 is it is characterised in that described emulsifying agent is selected from dehydration mountain
Pears alcohol laurate, polyoxyethylene laurel ether, AEO, polyoxyethylene monopalmitate and polyoxyethylene caster
One or more mixture of oil；Described wetting agent is selected from lauryl sodium sulfate, Nonyl pheno, alkyl phenol
Polyoxyethylene formaldehyde condensation products sulfate, APES formaldehyde condensation products sulfat phosphate, styrene phenol first
Urea formaldehyde polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde condensate sulfonates,
One of dialkyl succinylsuccinate sulfonated ester, this disk SPAN, soil temperature TWEEN or more than one combination.
6. the composition pesticide of encapsulated form according to claim 3 is it is characterised in that described dispersant is selected from aromatic series
Sulfonate, acrylic acid and acrylic ester copolymers, formaldehyde condensate sulfonate, copolymer-maleic anhydride sodium salt, polymerization of carboxylic acid sodium salt
Class, styrene alkyl polyoxyethylene ether phosphate, naphthalenesulfonic acid-formaldehyde condensate, triphenyl vinyl phenol polyethenoxy ether class and spread out
Biological esters, fatty alcohol polyethenoxy ether class, APES class, macromolecule EO-PO block copolymer, sulfomethylated lignin
Hydrochlorate, alkylphenol-polyethenoxy formaldehyde condensation products sulfate, APES formaldehyde condensation products sulfat phosphate, benzene
Phenol ethylene formaldehyde resin polyoxyethylene ether phosphate salt, styryl phenol polyethenoxy polyethenoxy ether, alkyl naphthalene formaldehyde contracting
Compound sulfonate, macromolecule dredge one or more of dress copolymer, polymerization of carboxylic acid salt of type；Described initiator is selected from salt
Acid, glacial acetic acid, fatty glyceride, lactolactone and the combination of amino acid ammonium chloride, ethylenediamine, 1- octyne -3- alcohol, triethylamine,
A kind of or arbitrarily several combination of glyceride lactate, triethanolamine, acid regulator or alkaline conditioner.
7. the composition pesticide of encapsulated form according to claim 3 is it is characterised in that described filler is selected from modified water-soluble
Starch, cellulose ether and its derivative, aluminium-magnesium silicate, kaolin, diatomite, attapulgite, glucose, precipitated calcium carbonate, white
One of carbon black, inorganic salts；Described stabilizer is selected from epoxidized soybean oil, 2,6- toluene di-tert-butyl phenol, butylhydroxy fennel
One or more of fragrant ether, triphenyl phosphite and potassium dihydrogen phosphate mixture；Described curing agent is selected from following one kind or one
Plant above composition：Double bond containing alcohol ether sulfosuccinates sodium salt, allyl alcohol ether sulfate, allyl ether hydroxypropanesulfonic acid
Sodium, sodium vinyl sulfonate, alkyl phenol allyl polyether sulfate acrylamido sodium isopropyl xanthate, 2- allyl ether 3- base
Propane -1- sodium sulfonate and allyl polyether sulfate；Described solvent be selected from methyl esters soybean oil, corn methyl esters oil, methyl esters palm oil,
One of methyl esters coconut oil, turpentine-based vegetable oil and fatty acid ester；Or toluene, acetone, isopropanol, chloroform, ethanol, first
One of alcohol, hexamethylene or two or more any mixing；Preferably methyl esters soybean oil, methyl esters palm oil or turpentine-based vegetable oil.
8. the composition pesticide of encapsulated form according to claim 3 is it is characterised in that described auxiliary addition agent is selected from bonding
The combination of one or more of agent, disintegrant, pH adjusting agent, sterilization antiseptic, defoamer, antifreeze, thickener；Wherein institute
The binding agent stated be selected from polyvinyl alcohol, gelatin, Arabic gum, xanthans, Sodium Polyacrylate, sodium alginate, starch, cellulose or
Cellulose derivative, preferred cellulose or cellulose derivative；Disintegrant is selected from aluminium-magnesium silicate, polyethylene glycol PEG, modified shallow lake
One kind of powder, inorganic salts, White Carbon black or silica gel；Described pH acid-base modifier is selected from glacial acetic acid, hydrochloric acid, ammoniacal liquor, monoethanolamine, three second
One of hydramine；Described sterilization antiseptic is selected from one of potassium sorbate, Sodium Benzoate, formaldehyde or OIT；Institute
State defoamer and be selected from natural oil, polyethers defoamer, higher alcohols, one kind of organic silicon defoamer；Described antifreeze is selected from third
Glycol or ethylene glycol；Described thickener is selected from xanthans, carragheen, pectin, agar, algin or sodium carboxymethylcellulose.
9. the composition pesticide of encapsulated form according to claim 1 is it is characterised in that described encapsulated form hangs for micro-capsule
Floating agent, micro-capsule suspension emulsion, microcapsulated granule, microcapsule suspension-suspendinagent agent, microcapsule suspension-aqueous emulsion or microcapsule suspension-suspension emulsion.
10. the composition pesticide of encapsulated form according to claim 9 is it is characterised in that hang in microcapsule suspending agent, micro-capsule
In emulsion or microcapsulated granule, the capsule-core of described encapsulated form comprises the mixture of active ingredient trefanocide and pendimethalin；Or
First prepare the packing containing active ingredient trefanocide or pendimethalin respectively, then by two kinds of packings in two kinds of active ingredients ratio
The micro-capsule part of mixing composition microcapsule suspending agent, micro-capsule suspension emulsion or microcapsulated granule；In microcapsule suspension-suspendinagent agent, micro-capsule
In suspension-aqueous emulsion or microcapsule suspending agent-suspension emulsion, first prepare the micro-capsule containing active ingredient trefanocide, by active ingredient two
First penta spirit is prepared into suspension, emulsion or suspended emulsion.
The composition pesticide of 11. encapsulated forms according to any one of claim 1～10 prevents and treats farming in agriculture field
The purposes of thing weeds.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610640964.1A CN106376561A (en) | 2016-08-07 | 2016-08-07 | Microcapsule type pesticide composition |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201610640964.1A CN106376561A (en) | 2016-08-07 | 2016-08-07 | Microcapsule type pesticide composition |
Publications (1)
| Publication Number | Publication Date |
|---|---|
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Family
ID=57916676
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|---|---|---|---|
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2019043868A (en) * | 2017-08-31 | 2019-03-22 | アース製薬株式会社 | Method for enhancing weeding activity of acetic acid, and acetic acid-containing herbicide |
| CN111011373A (en) * | 2019-12-26 | 2020-04-17 | 安徽云中生态农业开发有限公司 | Composite pesticide for controlling broccoli |
| CN112790199A (en) * | 2019-11-14 | 2021-05-14 | 兰州大学 | Botanical insecticide for preventing and treating corn weevil and preparation process thereof |
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| CN105532658A (en) * | 2015-08-02 | 2016-05-04 | 江苏辉丰农化股份有限公司 | Encapsulated pesticide composition |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2019043868A (en) * | 2017-08-31 | 2019-03-22 | アース製薬株式会社 | Method for enhancing weeding activity of acetic acid, and acetic acid-containing herbicide |
| CN112790199A (en) * | 2019-11-14 | 2021-05-14 | 兰州大学 | Botanical insecticide for preventing and treating corn weevil and preparation process thereof |
| CN111011373A (en) * | 2019-12-26 | 2020-04-17 | 安徽云中生态农业开发有限公司 | Composite pesticide for controlling broccoli |
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Application publication date: 20170208 |