CN107969421A - A kind of dispersible oil-suspending agent of glufosinate-ammonium and preparation method thereof - Google Patents

A kind of dispersible oil-suspending agent of glufosinate-ammonium and preparation method thereof Download PDF

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CN107969421A
CN107969421A CN201710381663.6A CN201710381663A CN107969421A CN 107969421 A CN107969421 A CN 107969421A CN 201710381663 A CN201710381663 A CN 201710381663A CN 107969421 A CN107969421 A CN 107969421A
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glufosinate
oil
ammonium
agent
suspending agent
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CN107969421B (en
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倪新荣
刘艳秋
李燕文
徐良
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NANJING TEVA-CHEM Co Ltd
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NANJING TEVA-CHEM Co Ltd
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    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, 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
    • A01N25/02Biocides, 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 containing liquids as carriers, diluents or solvents
    • A01N25/04Dispersions, emulsions, suspoemulsions, suspension concentrates or gels
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N25/00Biocides, 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
    • A01N25/30Biocides, 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 characterised by the surfactants
    • AHUMAN NECESSITIES
    • A01AGRICULTURE; FORESTRY; ANIMAL HUSBANDRY; HUNTING; TRAPPING; FISHING
    • A01NPRESERVATION OF BODIES OF HUMANS OR ANIMALS OR PLANTS OR PARTS THEREOF; BIOCIDES, e.g. AS DISINFECTANTS, AS PESTICIDES OR AS HERBICIDES; PEST REPELLANTS OR ATTRACTANTS; PLANT GROWTH REGULATORS
    • A01N57/00Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds
    • A01N57/18Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds
    • A01N57/20Biocides, pest repellants or attractants, or plant growth regulators containing organic phosphorus compounds having phosphorus-to-carbon bonds containing acyclic or cycloaliphatic radicals
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C303/00Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides
    • C07C303/32Preparation of esters or amides of sulfuric acids; Preparation of sulfonic acids or of their esters, halides, anhydrides or amides of salts of sulfonic acids
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C309/00Sulfonic acids; Halides, esters, or anhydrides thereof
    • C07C309/01Sulfonic acids
    • C07C309/02Sulfonic acids having sulfo groups bound to acyclic carbon atoms
    • C07C309/03Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton
    • C07C309/17Sulfonic acids having sulfo groups bound to acyclic carbon atoms of an acyclic saturated carbon skeleton containing carboxyl groups bound to the carbon skeleton
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C67/00Preparation of carboxylic acid esters
    • C07C67/08Preparation of carboxylic acid esters by reacting carboxylic acids or symmetrical anhydrides with the hydroxy or O-metal group of organic compounds
    • CCHEMISTRY; METALLURGY
    • C07ORGANIC CHEMISTRY
    • C07CACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C69/00Esters of carboxylic acids; Esters of carbonic or haloformic acids
    • C07C69/52Esters of acyclic unsaturated carboxylic acids having the esterified carboxyl group bound to an acyclic carbon atom
    • C07C69/593Dicarboxylic acid esters having only one carbon-to-carbon double bond
    • C07C69/60Maleic acid esters; Fumaric acid esters

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • General Health & Medical Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Pest Control & Pesticides (AREA)
  • Engineering & Computer Science (AREA)
  • Dentistry (AREA)
  • Wood Science & Technology (AREA)
  • Zoology (AREA)
  • Environmental Sciences (AREA)
  • Plant Pathology (AREA)
  • Agronomy & Crop Science (AREA)
  • Toxicology (AREA)
  • Dispersion Chemistry (AREA)
  • Agricultural Chemicals And Associated Chemicals (AREA)

Abstract

The invention discloses a kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 5 30%, emulsifying agent 5 20%, wetting dispersing agent 1 5%, thixotropic agent 0.1 5%, surplus is decentralized medium.The dispersible oil-suspending agent preparation method step of glufosinate-ammonium is as follows:(1) emulsifying agent, the wetting dispersing agent to mix with oil phase, decentralized medium are mixed and be uniformly dispersed;(2) Glufosinate-ammonium is added;(3) thixotropic agent is added, high speed shear is carried out after being stirred;(4) it is sanded under abrasive media, grinds 1 2h, particle diameter D90 is below 5 microns.The dispersible oil-suspending agent of glufosinate-ammonium of the present invention, room temperature and heat storage condensate oil are less, are placed at room temperature through shaking resilient, no knot bottom phenomenon;With good heat storage stability and low-temperature stability, said preparation safety and environmental protection, resistance of rainwater washing against, good drug efficacy, lasting period length.

Description

A kind of dispersible oil-suspending agent of glufosinate-ammonium and preparation method thereof
Technical field
The present invention relates to pesticide field, is specifically related to dispersible oil-suspending agent of a kind of glufosinate-ammonium and preparation method thereof.
Background technology
Glufosinate-ammonium category phosphonic acid herbicide, is glutamine synthetase inhibitor, has the non-selective of part systemic action Contact weedicide.Glufosinate-ammonium toxicity is low, be easy to degraded in the soil, to crop safety, be not easy drift, herbicidal spectrum is wide, activity is high, Good absorbing, environmental pressure are small, weed eradication is rapid, can quickly kill more than 100 kinds of grass family and broad leaved weed.Meanwhile and generation The second largest genetically modified crops herbicide-tolerant in boundary, generally should in countries such as Japan, South Korea, Southeast Asia, America, Europe With.At home, with the large area of glyphosate, reuse, already lead to a large amount of weeds and produce resistances, and paraquat aqua by It is too strong in toxicity, stopped using in July, 2016, popular anchor man of the glufosinate-ammonium into paraquat.It can be seen from the above that paraquat water After agent disabling, the prospect of glufosinate-ammonium is very wide.
Over the past two years, action of each means of agricultural production enterprise in glufosinate-ammonium was frequent.Recognize from Chinese pesticide Information Network, 2012 The registration card of year glufosinate-ammonium product only has 11, increases 102 within 2016, wherein, active compound 23,73 (70, preparation Aqua, 3 soluble granules), it is seen that register most for glufosinate-ammoniumaqua aqua.But glufosinate-ammoniumaqua aqua have two aspect restriction because Element, the first glufosinate-ammonium belong to salt in itself, cannot be coexisted in conventional surfactant in aqueous systems, and auxiliary agent is matched and is required It is higher.Second glufosinate-ammoniumaqua aqua is higher to the susceptibility of environment, and temperature and humidity has a great impact the drug effect of glufosinate-ammonium.It is wet When spending relatively low, plant epidermis drying stomata is closed, leaf rolling, is unfavorable for the absorption of glufosinate-ammonium;Under cryogenic, glufosinate-ammonium Reduced by the ability of cuticula and cell membrane, so as to influence herbicidal effect.When environment is unfavorable, glufosinate-ammonium herbicidal effect is paid no attention to Think.
Dispersible oil-suspending agent decentralized medium is oily, and mostly mineral oil or vegetable oil, document report vegetable oil and pesticide Mixture spray after be not easy to be lost in by rain drop erosion, remain to keep good drug effect under conditions of arid, have good Penetration, while oil than water has stronger plate-out ability, so as to add the covering surface to plant, especially wax-like blade is planted Thing.Oils is had made intensive studies as pesticide spray auxiliary agent both at home and abroad, oils can be as the effect of the synergist of herbicide Mechanism is commonly considered as strengthening deposition, delay, spread, infiltration and the absorption of spray droplet.Vegetable oil can reduce air and liquid Interface on drop surface tension, reduce contact angle, strengthen the wetability of pesticide, extension of the increase pesticide droplet in leaf surface Area;Increase the viscosity of liquid, liquid is easily got adhered in leaf surface of plant, resistance of rainwater washing against;Dissolving destroys plant part Wax coat or cuticula, improve its penetrating power, reduce stomatal conductance, promote absorption of the plant to pesticide, so as to improve pesticide Utilization rate.In addition vegetable oil can prevent the too fast drying of drop, so as to strengthen stomata and cuticula to farm chemical ingredients in drop Absorb.The dispersible oil-suspending agent of glufosinate-ammonium is processed into using vegetable oil as decentralized medium, the advantage of vegetable oil can be given full play to, again Environmentally sensitive this higher defect of degree of glufosinate-ammonium can be made up so as to improve drug effect.
But vegetable oil still suffers from some shortcomings in itself as the common decentralized medium of dispersible oil-suspending agent:Activities of Some Plants oil is molten Solution property is poor, volatility is high, emulsification is difficult, cost is higher, limits the popularization and application of vegetable oil solvent to a certain degree;Vegetable oil into Divide complexity not easy to control, performance is poor compared with organic solvent stability, and different vegetable oil solidification points differ, and are easily planted by separate sources The influence of thing, accumulating condition;Therefore, the low-temperature stability and emulsification point of the source of vegetable oil and species to dispersible oil-suspending agent Scattered property has a great influence.These are an important factor for dispersible oil-suspending agent of obstruction develop, therefore are opened in dispersible oil suspending agent preparation The purposes that preparation should be also combined during hair carries out the screening of oils.
The technical requirements that the particularity of Glufosinate-ammonium prepares dispersible oil-suspending agent are higher, by literature search, rarely have grass The document report of the dispersible oil-suspending agent preparation processing of ammonium phosphine.By many experiments, the dispersible oil-suspending agent system of glufosinate-ammonium is found It is difficult to solve there are problems in standby:(1) glufosinate-ammonium belongs to salt in itself, and selectable auxiliary agent species is considerably less in processing, Components do match requires very high between system;(2) vegetable oil comparison of ingredients is complicated, and Glufosinate-ammonium is processing dispersible oil-suspending agent When it is more demanding to plant oil decentralized medium, compounded by screening not decentralized medium of the same race, adjust dispersible oil suspensions system Viscosity, solidification point and HLB value, reduce low temperature effect and solve decentralized medium being not easy the problem that emulsifies;(3) glufosinate-ammonium is dispersible Preparation condensate oil is very much (even more commonly greater than 20%) after the storage for a long time of oil-suspending agent preparation, when room temperature or heat storage easy retrogradation and Tie bottom;(4) preparation places easily caking for a long time.
The content of the invention
Above-mentioned technical problem is run into order to overcome in the outstanding preparation of the dispersible oil of glufosinate-ammonium, the present invention is suitably helped by selection Agent system and the decentralized medium system and processing technology to match, a kind of successful formulation dispersible oil-suspending agent of glufosinate-ammonium.Should Preparation has room temperature and heat storage condensate oil less, is placed at room temperature through shaking resilient, no knot bottom phenomenon.
Technical solution:The dispersible oil-suspending agent of a kind of glufosinate-ammonium of the present invention, by the material of following percentage by weight Composition:Glufosinate-ammonium 5-30%, emulsifying agent 5-20%, wetting dispersing agent 1-5%, thixotropic agent 0.1-5%, surplus are decentralized medium.
The emulsifying agent is selected from fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, triphen Ethyl -phenol polyoxyethylene ether, oleic acid polyoxyethylene, sorbitan fatty acid ester polyoxyethylene ether, propane diols polyoxyethylene One or more in polyoxypropylene block polymer, APES formaldehyde condensation product, calcium dodecyl benzene sulfonate The mixture of arbitrary proportion combination.Preferred emulsifier triphenoethyl benzene phenol polyethenoxy ether, the contracting of alkylphenol polyoxyethylene ether formaldehyde The one or two of compound.In triphenoethyl benzene phenol polyethenoxy ether, APES formaldehyde condensation product monomer structure With multiple benzene ring structures, phenyl ring forms pi-pi bond with pesticide particle planes of molecules, the two is firmly combined together, and makes pesticide It is particle stabilized scattered.
The wetting dispersing agent be selected from alkylphenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether sulfuric acid, Alkylphenol polyoxyethylene ether carboxylate, APES formaldehyde condensation products sulfat, fatty alcohol polyoxyethylene ether phosphoric acid Ester, aliphatic alcohol polyethenoxy ether carboxylate, polyoxyethylene alkyl ether sulfate salt, triphenoethyl benzene phenol polyethenoxy ether phosphoric acid Ester, dodecyl benzene sulfonic acid amine salt, the different dioctyl sodium sulfosuccinate of maleic acid, lignosulfonates, naphthalene sulfonate, self-control dispersant The mixture of one or more of arbitrary proportions combination in A.It is preferred that wetting dispersing agent makes dispersant A by oneself.The advantages of dispersant A, exists In the anionic dispersing agents that oiliness group is larger, lipophile can be good at more by force and nonionic surfactant collocation oil emulsion Sour methyl esters.It is long-term that the collocation of dispersant A and nonionic surfactant can effectively solve the dispersible oil-suspending agent preparation of glufosinate-ammonium The problems such as preparation condensate oil is many after storage, and easy retrogradation and knot bottom and preparation place easy caking for a long time when room temperature or heat are store.
The preparation process of A is as follows:Nonylphenol polyoxyethylene ether (NP-4) is obtained along succinic acid with maleic acid anhydride reactant Nonylphenol polyoxyethylene ether monoesters, along succinic acid nonylphenol polyoxyethylene ether monoesters and fatty acid dehydration generation dibasic acid esters, then With sodium hydrogensulfite sulfonation up to dispersant A.Its reaction equation is as follows:
One or more of the thixotropic agent in white carbon, organobentonite, rilanit special, polyamide wax are appointed The mixture of meaning ratio combination.
The decentralized medium is selected from plant oil such as soybean oil, peanut oil, rapeseed oil, corn oil, castor oil, turpentine Oil, improved plant oils such as methyl oleate, biodiesel, epoxidized soybean oil, one in mineral oils such as petroleum hydrocarbon, solvent naphtha Kind or the mixture of several arbitrary proportions combination.
The present invention also provides a kind of dispersible oil-suspending agent preparation method step of glufosinate-ammonium is as follows:(1) by emulsifying agent and oil Wetting dispersing agent, the decentralized medium to mix is mixed and is uniformly dispersed;(2) Glufosinate-ammonium is added;(3) thixotropic agent, stirring are added High speed shear is carried out after mixing;(4) it is sanded under abrasive media, grinds 1-2h, particle diameter D90 is below 5 microns.
The dispersible oil-suspending agent of glufosinate-ammonium of the present invention can be applied to prevent and kill off lady's-grass, barnyard grass, cogongrass, the rhizome of nutgrass flatsedge, dog In root of the tooth, Amaranthus retroflexus.
Beneficial effect:The dispersible oil-suspending agent of glufosinate-ammonium of the present invention, room temperature and heat storage condensate oil are less, are placed in room temperature It is lower through shake resilient, it is no knot bottom phenomenon;With good heat storage stability and low-temperature stability, said preparation safety collar Guarantor, resistance of rainwater washing against, good drug efficacy, lasting period length.
Embodiment
In order to deepen the understanding of the present invention, below in conjunction with embodiment, the invention will be further described, these implementations Example is only used for explaining the present invention, is not intended to limit the scope of the present invention..
Embodiment 1
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 15%, emulsifying agent 12%th, wetting dispersing agent 3%, thixotropic agent 4%, surplus are decentralized medium.
By 4% triphenoethyl benzene phenol polyethenoxy ether, 4% propane diols polyoxyethylene polyoxypropylene block polymer, 4%0 Dialkyl benzene sulfonic acids calcium, 3% alkylphenol polyoxyethylene ether carboxylate, 20% solvent naphtha, the mixing of surplus methyl oleate are uniformly dispersed; Add 15% Glufosinate-ammonium;3.5% gas-phase silica, 0.5% organobentonite are added, carries out cutting at a high speed after being stirred Cut;It is sanded under abrasive media, grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 2
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 15%, emulsifying agent 12%th, wetting dispersing agent 3%, thixotropic agent 4%, surplus are decentralized medium.
By 3% APES formaldehyde condensation product, 4% triphenoethyl benzene phenol polyethenoxy ether, 5% dodecyl Benzene sulfonic acid calcium, 3% dispersant A are mixed and are uniformly dispersed with 20% epoxidized soybean oil, surplus methyl oleate;Add 15% glufosinate-ammonium original Medicine;3.5% gas-phase silica, 0.5% organobentonite are added, high speed shear is carried out after being stirred;Under abrasive media into Row is sanded, and grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 3
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 18%, emulsifying agent 12%th, wetting dispersing agent 3%, thixotropic agent 4%, surplus are decentralized medium.
By 4% triphenoethyl benzene phenol polyethenoxy ether, 4% APES formaldehyde condensation product, 4% dodecyl Benzene sulfonic acid calcium, the different dioctyl sodium sulfosuccinate of 3% maleic acid are mixed with methyl oleate and are uniformly dispersed;Add 18% Glufosinate-ammonium; 3.5% gas-phase silica, 0.5% organobentonite are added, high speed shear is carried out after being stirred;Sand is carried out under abrasive media Mill, grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 4
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 18%, emulsifying agent 12%th, wetting dispersing agent 3%, thixotropic agent 4%, surplus are decentralized medium.
By 4% triphenoethyl benzene phenol polyethenoxy ether, 4% APES formaldehyde condensation product, 4% dodecyl Benzene sulfonic acid calcium, 3% dispersant A are mixed and are uniformly dispersed with 20% solvent naphtha, surplus methyl oleate;Add 18% Glufosinate-ammonium; 3.5% gas-phase silica, 0.5% organobentonite are added, high speed shear is carried out after being stirred;Sand is carried out under abrasive media Mill, grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 5
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 18%, emulsifying agent 12%th, wetting dispersing agent 3%, thixotropic agent 4%, surplus are decentralized medium.
By 3% APES formaldehyde condensation product, 4% triphenoethyl benzene phenol polyethenoxy ether, 5% dodecyl Benzene sulfonic acid calcium, 3% dispersant A are mixed and are uniformly dispersed with 20% epoxidized soybean oil, surplus methyl oleate;Add 18% glufosinate-ammonium original Medicine;3.5% gas-phase silica, 0.5% organobentonite are added, high speed shear is carried out after being stirred;Under abrasive media into Row is sanded, and grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 6
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 30%, emulsifying agent 15%th, wetting dispersing agent 4%, thixotropic agent 2%, surplus are decentralized medium.
By 4% triphenoethyl benzene phenol polyethenoxy ether, 4% propane diols polyoxyethylene polyoxypropylene block polymer, 3% alkane Base phenol polyethenoxy ether formaldehyde condensation products, 4% calcium dodecyl benzene sulfonate, 4% dispersant A and 15% solvent naphtha, surplus oleic acid Methyl esters mixing is uniformly dispersed;Add 30% Glufosinate-ammonium;2% gas-phase silica is added, high speed shear is carried out after being stirred; It is sanded under abrasive media, grinds 1-2h, particle diameter D90 is below 5 microns.
Embodiment 7
A kind of dispersible oil-suspending agent of glufosinate-ammonium, by the material composition of following percentage by weight:Glufosinate-ammonium 30%, emulsifying agent 15%th, wetting dispersing agent 4%, thixotropic agent 1%, surplus are decentralized medium.
By 4% triphenoethyl benzene phenol polyethenoxy ether, 4% propane diols polyoxyethylene polyoxypropylene block polymer, 3% alkane Base phenol polyethenoxy ether formaldehyde condensation products, 4% calcium dodecyl benzene sulfonate, 4% dispersant A and 10% solvent naphtha, 5% epoxy are big Soya-bean oil, the mixing of surplus methyl oleate are uniformly dispersed;Add 30% Glufosinate-ammonium;1% gas-phase silica is added, after being stirred Carry out high speed shear;It is sanded under abrasive media, grinds 1-2h, particle diameter D90 is below 5 microns.
The dispersible oil-suspending agent performance indicator measurement result such as following table of embodiment 1-7 glufosinate-ammoniums:
Index of correlation assay method is according to the dispersible oily Suspension index of GB/T 28155-2011 nicosulfurons in table.
Suspensibility:According to GB/T 14825-2006 agricultural chemicals suspension agent assay methods.Appropriate amount of sample is weighed, input fills In the graduated cylinder of 250mL standard hard waters, turn upside down in 2min 30 times, then stood in the thermostat for filling 25 DEG C of water 30min.9/10 (i.e. 225mL) suspension of content is pumped, not shake or stir the sediment in graduated cylinder.By graduated cylinder bottom It is m that 25mL suspension, which is transferred to known quality,1Culture dish, dried in 50 DEG C of baking ovens to constant, weigh residue quality m2, Its specimen suspension rate formula is as follows:
Dispersion stabilization:Dispersed simple and easy method is measured using the national analysis of agricultural drugs committee (CIPAC) seminar DAPF, Step is as follows:Add 98mL deionized waters in 100mL graduated cylinders, claim in 2g sample introduction cylinders, overturn 10 times, about 2s, remembers every time Volume of sediment when recording 30min.Microprecipitation is denoted as dispersion performance qualification.
Heat storage stability:Carried out by GB/T19136-2003-2.3 methods, every batch of about 15g samples are sealed in 50mL ampoules In bottle, it is placed in (54 ± 2) DEG C constant temperature oven, is taken out after storing 14d, sample active constituent content and suspension before and after being store to heat Rate is detected analysis, and resolution ratio is not more than 5%, and suspensibility meets index for qualification.
Low-temperature stability:Carried out by GB/T19137-2003 suspension formulations method, take the sample of 80mL to be placed in 100mL beakers In, it is cooled to ((0 scholar 2) DEG C, holding 1h, at interval of 15min stirrings once, each 15s, observation appearance whether there is in refrigerator Change.Beaker is put back into refrigerator, (after (0 scholar 2) DEG C continues placement 7d, 7d, beaker is being taken out, is being recovered to room temperature, test sieve Analysis, suspensibility or other necessary physical and chemical indexes.
Careless ammonium in above table it can be seen from each dispersible oil-suspending agent performance indicator of glufosinate-ammonium prepared by the present invention The dispersible oil-suspending agent of phosphine largely all has good dispersion stabilization, heat storage stability and low-temperature stability, and condensate oil is few, only There is a small amount of knot bottom phenomenon, easily shaken up after long-term placement, without caking phenomenon.
Embodiment 9
Field control effectiveness test:
Reagent agent:Four kinds of dispersible oil-suspending agents of glufosinate-ammonium in embodiment 2,5,6,7.
Comparison medicament:Commercially available 18% glufosinate-ammonium (original powder) aqua
Control object:The weeds such as lady's-grass, barnyard grass, cogongrass, the rhizome of nutgrass flatsedge, Bermuda grass, Amaranthus retroflexus.
Test method:According to the area of experimental plot, the good various medicaments of precise, and it is watered dilution.Cell is area 20m2Rectangle, using random district's groups arrange, plug in label, and on board mark processing number and repeated number, be repeated 2 times.Dispenser Sprayed using the 3WDB-16 type knapsack electric sprayers with Fan spray head, operating pressure 0.2-0.4mpa, has often sprayed one Sprayer is cleaned after kind medicament, sprayer is dripped using mist, is got it filled by each processing dosage, water consumption is 30L/ mus, in gentle breeze Under the conditions of spray.
After experiment weeds death condition, and the activity of weeding of more various medicaments are observed in 14d.
Preparation of the embodiment of the present invention see the table below with contrast agents Herbicidal Testing Trials effect:
As seen from the above table, in glufosinate-ammonium effective ingredient consumption under 39.6g/ mus of usage amounts, embodiment 2,5,6,7 is dispersible 14d plants of preventive effects are all higher than 14d plants of preventive effects after the medicine of 18% glufosinate-ammoniumaqua aqua of contrast agents after the medicine of oil-suspending agent.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art Scholar can understand present disclosure and implement according to this, and it is not intended to limit the scope of the present invention, it is all according to the present invention The equivalent change or modification that Spirit Essence is made, should be covered by the protection scope of the present invention.

Claims (8)

1. a kind of dispersible oil-suspending agent of glufosinate-ammonium, it is characterised in that by the material composition of following percentage by weight:Glufosinate-ammonium 5- 30%, emulsifying agent 5-20%, wetting dispersing agent 1-5%, thixotropic agent 0.1-5%, surplus are decentralized medium;
The emulsifying agent is selected from fatty alcohol polyoxyethylene ether, castor oil polyoxyethylene ether, alkylphenol polyoxyethylene ether, three phenethyls Phenol polyoxyethylene ether, oleic acid polyoxyethylene, sorbitan fatty acid ester polyoxyethylene ether, propane diols polyoxyethylene polyoxy One or more in propylene block copolymer, APES formaldehyde condensation product, calcium dodecyl benzene sulfonate are any The mixture of ratio combination;
The wetting dispersing agent is selected from alkylphenol polyoxyethylene ether phosphate, alkylphenol polyoxyethylene ether sulfuric acid, alkyl Phenol polyethenoxy ether carboxylate, APES formaldehyde condensation products sulfat, aliphatic alcohol polyoxyvinethene phosphate, fat Fat alcohol polyethenoxy ether carboxylate, polyoxyethylene alkyl ether sulfate salt, triphenoethyl benzene phenol polyethenoxy ether phosphate, ten In the different dioctyl sodium sulfosuccinate of dialkyl benzene sulfonic acids amine salt, maleic acid, lignosulfonates, naphthalene sulfonate, self-control dispersant A The mixture of one or more of arbitrary proportion combinations;
The mixing of one or more of arbitrary proportions combination of the dispersant in vegetable oil, modified vegetable oil or mineral oil Thing.
2. the dispersible oil-suspending agent of glufosinate-ammonium according to claim 1, it is characterised in that the thixotropic agent is selected from hard charcoal The mixture of one or more of arbitrary proportions combination in black, organobentonite, rilanit special, polyamide wax.
3. the dispersible oil-suspending agent of glufosinate-ammonium according to claim 1, it is characterised in that the emulsifying agent is selected from triphen second One or both of base phenol polyoxyethylene ether, APES formaldehyde condensation product.
4. the dispersible oil-suspending agent of glufosinate-ammonium according to claim 1, it is characterised in that the wetting dispersing agent is selected from Make dispersant A by oneself, the molecular formula of the self-control dispersant is as follows:
5. the dispersible oil-suspending agent of glufosinate-ammonium according to claim 4, it is characterised in that the preparation of the self-control dispersant Technique is as follows:Nonylphenol polyoxyethylene ether is obtained along succinic acid nonylphenol polyoxyethylene ether monoesters with maleic acid anhydride reactant, Along succinic acid nonylphenol polyoxyethylene ether monoesters and fatty acid dehydration generation dibasic acid esters, then with sodium hydrogensulfite sulfonation, that is, score Powder A.
6. the dispersible oil-suspending agent of glufosinate-ammonium according to claim 1, it is characterised in that the vegetable oil for soybean oil, Peanut oil, rapeseed oil, corn oil, castor oil or turpentine oil, the improved plant oils are methyl oleate, biodiesel or epoxy Soybean oil, the mineral oils are petroleum hydrocarbon or solvent naphtha.
7. a kind of preparation method of the dispersible oil-suspending agent of glufosinate-ammonium, it is characterised in that comprise the following steps that:(1) by emulsifying agent, Wetting dispersing agent, the decentralized medium to mix with oil phase, which mixes, to be uniformly dispersed;(2) Glufosinate-ammonium is added;(3) thixotropic agent is added, High speed shear is carried out after being stirred;(4) it is sanded under abrasive media, grinds 1-2h, particle diameter D90 is below 5 microns.
8. a kind of application of the dispersible oil-suspending agent of glufosinate-ammonium, it is characterised in that the dispersible oil-suspending agent of glufosinate-ammonium is preventing and kill off horse Tang, the application of barnyard grass, cogongrass, the rhizome of nutgrass flatsedge, Bermuda grass, Amaranthus retroflexus.
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CN108849871B (en) * 2018-08-22 2021-02-23 苏州丰倍生物科技有限公司 Environment-friendly oil phase for dispersible oil suspending agent containing mesosulfuron-methyl and preparation method thereof
CN108849871A (en) * 2018-08-22 2018-11-23 苏州丰倍生物科技有限公司 Environment-friendly oil phase for dispersible oil suspending agent containing mesosulfuron-methyl and preparation method thereof
CN109006860A (en) * 2018-10-21 2018-12-18 江苏长青生物科技有限公司 Glufosinate-ammonium and the oily suspension herbicide of dicamba component and preparation method thereof
CN109169704A (en) * 2018-10-21 2019-01-11 江苏长青生物科技有限公司 A kind of oily suspension herbicide and preparation method thereof of glufosinate-ammonium and fluoroglycofen-ethyl combination
CN109221244A (en) * 2018-10-21 2019-01-18 江苏长青生物科技有限公司 Glufosinate-ammonium and the micro emulsion herbicide of fluoroglycofen-ethyl component and preparation method thereof
CN109463383A (en) * 2018-11-21 2019-03-15 江苏钟山化工有限公司 A kind of glufosinate-ammonium oil-suspending agent and preparation method thereof
CN109497058A (en) * 2018-12-04 2019-03-22 四川赛华睿科技有限责任公司 A kind of glyphosate synergist of effects enhancing and dose reducing
CN110105542A (en) * 2019-05-20 2019-08-09 南京太化化工有限公司 A kind of parents' oil base modified bisphenol A type epoxy resin surface activating agent and the preparation method and application thereof
CN110105542B (en) * 2019-05-20 2022-01-18 南京太化化工有限公司 Amphiphilic oil-based modified bisphenol A epoxy resin surfactant and preparation method and application thereof
CN113016824A (en) * 2019-12-09 2021-06-25 德强生物股份有限公司 Sucus subtilis dispersible oil suspending agent and preparation process thereof
CN112778994A (en) * 2020-12-31 2021-05-11 中海石油(中国)有限公司湛江分公司 High-temperature-resistant high-salt surfactant composition and preparation method and application thereof
CN112778994B (en) * 2020-12-31 2022-04-12 中海石油(中国)有限公司湛江分公司 High-temperature-resistant high-salt surfactant composition and preparation method and application thereof
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